data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Mulvey, R.E.' _publ_contact_author_email R.E.MULVEY@STRATH.AC.UK _publ_section_title ; N-Heterocyclic carbene stabilized adducts of alkyl magnesium amide, bisalkyl magnesium and Grignard reagents: Trapping oligomeric organo s-block fragments with NHCs ; _publ_contact_author_address ; WestCHEM, Department of Pure and Applied Chemistry, University of Strathclyde, Glasgow, G1 1XL, U.K. ; loop_ _publ_author_name A.R.Kennedy R.E.Mulvey S.Robertson # Attachment '- combined.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 775962' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H63 Mg N3' _chemical_formula_sum 'C40 H63 Mg N3' _chemical_formula_weight 610.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.7980(8) _cell_length_b 11.7552(5) _cell_length_c 17.4673(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3859.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7016 _cell_measurement_theta_min 2.4546 _cell_measurement_theta_max 29.1020 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95997 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16084 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 29.08 _reflns_number_total 7556 _reflns_number_gt 5867 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ADDSYM reports potential centre of symmetry. This is not supported by the cell contents. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.35(19) _refine_ls_number_reflns 7556 _refine_ls_number_parameters 419 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.75387(3) 0.54558(5) 0.73501(4) 0.02125(13) Uani 1 1 d . . . C40 C 0.77045(10) 0.72375(16) 0.74579(14) 0.0301(5) Uani 1 1 d . . . H40A H 0.8094(12) 0.7509(19) 0.7191(13) 0.052(7) Uiso 1 1 d . . . H40B H 0.7847(12) 0.737(2) 0.7961(15) 0.057(7) Uiso 1 1 d . . . C41 C 0.70580(9) 0.79688(14) 0.72577(12) 0.0274(4) Uani 1 1 d . . . H41A H 0.6868 0.7708 0.6759 0.033 Uiso 1 1 calc R . . H41B H 0.6685 0.7831 0.7647 0.033 Uiso 1 1 calc R . . C42 C 0.71876(9) 0.92432(14) 0.72082(11) 0.0243(4) Uani 1 1 d . . . H42A H 0.7500 0.9397 0.6764 0.029 Uiso 1 1 calc R . . H42B H 0.7444 0.9490 0.7674 0.029 Uiso 1 1 calc R . . C43 C 0.65152(10) 0.99518(17) 0.71276(12) 0.0340(5) Uani 1 1 d . . . H43A H 0.6644 1.0752 0.7053 0.051 Uiso 1 1 calc R . . H43B H 0.6227 0.9876 0.7592 0.051 Uiso 1 1 calc R . . H43C H 0.6242 0.9684 0.6685 0.051 Uiso 1 1 calc R . . N1 N 0.66056(6) 0.46744(12) 0.73617(9) 0.0216(3) Uani 1 1 d . . . C10 C 0.62061(10) 0.46159(17) 0.66429(10) 0.0251(4) Uani 1 1 d . . . C11 C 0.55748(10) 0.54379(19) 0.66412(11) 0.0340(5) Uani 1 1 d . . . H11A H 0.5756 0.6227 0.6606 0.041 Uiso 1 1 calc R . . H11B H 0.5280 0.5291 0.6182 0.041 Uiso 1 1 calc R . . C12 C 0.51110(9) 0.53302(16) 0.73506(13) 0.0348(5) Uani 1 1 d . . . H12A H 0.4875 0.4578 0.7354 0.042 Uiso 1 1 calc R . . H12B H 0.4738 0.5924 0.7343 0.042 Uiso 1 1 calc R . . C13 C 0.55655(11) 0.54619(18) 0.80678(11) 0.0320(5) Uani 1 1 d . . . H13A H 0.5266 0.5330 0.8526 0.038 Uiso 1 1 calc R . . H13B H 0.5750 0.6250 0.8094 0.038 Uiso 1 1 calc R . . C14 C 0.61960(10) 0.46216(16) 0.80747(11) 0.0244(4) Uani 1 1 d . . . C15 C 0.59514(12) 0.34091(18) 0.64377(12) 0.0362(5) Uani 1 1 d . . . H15A H 0.5546 0.3205 0.6762 0.054 Uiso 1 1 calc R . . H15B H 0.6340 0.2867 0.6522 0.054 Uiso 1 1 calc R . . H15C H 0.5807 0.3388 0.5899 0.054 Uiso 1 1 calc R . . C16 C 0.67286(11) 0.4981(2) 0.60099(11) 0.0349(5) Uani 1 1 d . . . H16A H 0.6866 0.5777 0.6089 0.052 Uiso 1 1 calc R . . H16B H 0.6499 0.4901 0.5509 0.052 Uiso 1 1 calc R . . H16C H 0.7153 0.4498 0.6029 0.052 Uiso 1 1 calc R . . C17 C 0.59144(11) 0.34153(18) 0.82740(12) 0.0330(5) Uani 1 1 d . . . H17A H 0.6302 0.2862 0.8226 0.049 Uiso 1 1 calc R . . H17B H 0.5530 0.3212 0.7921 0.049 Uiso 1 1 calc R . . H17C H 0.5734 0.3411 0.8800 0.049 Uiso 1 1 calc R . . C18 C 0.67036(11) 0.4959(2) 0.87154(11) 0.0352(5) Uani 1 1 d . . . H18A H 0.6862 0.5745 0.8637 0.053 Uiso 1 1 calc R . . H18B H 0.7116 0.4450 0.8713 0.053 Uiso 1 1 calc R . . H18C H 0.6458 0.4901 0.9209 0.053 Uiso 1 1 calc R . . C1 C 0.86017(8) 0.45966(13) 0.72007(10) 0.0173(3) Uani 1 1 d . . . N2 N 0.90071(7) 0.44614(11) 0.65610(8) 0.0163(3) Uani 1 1 d . . . N3 N 0.90559(8) 0.43156(12) 0.77762(8) 0.0184(3) Uani 1 1 d . . . C2 C 0.96915(9) 0.41094(15) 0.67370(10) 0.0221(4) Uani 1 1 d . . . H2A H 1.0066 0.3965 0.6385 0.027 Uiso 1 1 calc R . . C3 C 0.97218(9) 0.40124(15) 0.75041(9) 0.0206(4) Uani 1 1 d . . . H3A H 1.0121 0.3782 0.7800 0.025 Uiso 1 1 calc R . . C23 C 0.87369(9) 0.45886(16) 0.57891(10) 0.0202(4) Uani 1 1 d . . . C24 C 0.84743(9) 0.36074(17) 0.54279(10) 0.0236(4) Uani 1 1 d . . . C25 C 0.82070(10) 0.37452(19) 0.46836(11) 0.0289(5) Uani 1 1 d . . . H25A H 0.8031 0.3102 0.4414 0.035 Uiso 1 1 calc R . . C26 C 0.81955(10) 0.47973(19) 0.43384(11) 0.0337(5) Uani 1 1 d . . . H26A H 0.8000 0.4876 0.3840 0.040 Uiso 1 1 calc R . . C27 C 0.84643(11) 0.57357(19) 0.47091(11) 0.0330(5) Uani 1 1 d . . . H27A H 0.8458 0.6452 0.4458 0.040 Uiso 1 1 calc R . . C28 C 0.87453(10) 0.56589(16) 0.54444(10) 0.0241(4) Uani 1 1 d . . . C29 C 0.84984(10) 0.24437(17) 0.57925(11) 0.0300(5) Uani 1 1 d . . . H29A H 0.8575 0.2549 0.6355 0.036 Uiso 1 1 calc R . . C30 C 0.91253(11) 0.17562(19) 0.54786(14) 0.0452(6) Uani 1 1 d . . . H30A H 0.9570 0.2166 0.5578 0.068 Uiso 1 1 calc R . . H30B H 0.9067 0.1651 0.4926 0.068 Uiso 1 1 calc R . . H30C H 0.9141 0.1012 0.5731 0.068 Uiso 1 1 calc R . . C31 C 0.78048(11) 0.17780(19) 0.56853(14) 0.0439(6) Uani 1 1 d . . . H31A H 0.7406 0.2226 0.5884 0.066 Uiso 1 1 calc R . . H31B H 0.7834 0.1056 0.5964 0.066 Uiso 1 1 calc R . . H31C H 0.7730 0.1626 0.5139 0.066 Uiso 1 1 calc R . . C32 C 0.90911(11) 0.66749(16) 0.58225(11) 0.0289(4) Uani 1 1 d . . . H32A H 0.9077 0.6551 0.6389 0.035 Uiso 1 1 calc R . . C33 C 0.87052(15) 0.78014(18) 0.56512(13) 0.0495(6) Uani 1 1 d . . . H33A H 0.8199 0.7723 0.5775 0.074 Uiso 1 1 calc R . . H33B H 0.8758 0.7988 0.5107 0.074 Uiso 1 1 calc R . . H33C H 0.8913 0.8411 0.5962 0.074 Uiso 1 1 calc R . . C34 C 0.98758(12) 0.6745(2) 0.55799(15) 0.0503(6) Uani 1 1 d . . . H34A H 1.0116 0.6029 0.5706 0.075 Uiso 1 1 calc R . . H34B H 1.0107 0.7373 0.5852 0.075 Uiso 1 1 calc R . . H34C H 0.9905 0.6878 0.5027 0.075 Uiso 1 1 calc R . . C35 C 0.88311(9) 0.42391(16) 0.85755(9) 0.0200(4) Uani 1 1 d . . . C36 C 0.85785(9) 0.31839(16) 0.88242(10) 0.0238(4) Uani 1 1 d . . . C37 C 0.83203(10) 0.31351(19) 0.95699(10) 0.0303(5) Uani 1 1 d . . . H37A H 0.8141 0.2436 0.9763 0.036 Uiso 1 1 calc R . . C38 C 0.83195(11) 0.4083(2) 1.00336(11) 0.0358(5) Uani 1 1 d . . . H38A H 0.8128 0.4035 1.0536 0.043 Uiso 1 1 calc R . . C39 C 0.85955(10) 0.51088(19) 0.97752(11) 0.0301(5) Uani 1 1 d . . . H39A H 0.8602 0.5749 1.0107 0.036 Uiso 1 1 calc R . . C50 C 0.88626(9) 0.52090(16) 0.90338(10) 0.0240(4) Uani 1 1 d . . . C51 C 0.85597(10) 0.21459(16) 0.83130(11) 0.0280(4) Uani 1 1 d . . . H51A H 0.8917 0.2265 0.7896 0.034 Uiso 1 1 calc R . . C52 C 0.78297(11) 0.20327(17) 0.79350(13) 0.0346(5) Uani 1 1 d . . . H52A H 0.7722 0.2729 0.7649 0.052 Uiso 1 1 calc R . . H52B H 0.7467 0.1913 0.8330 0.052 Uiso 1 1 calc R . . H52C H 0.7833 0.1383 0.7583 0.052 Uiso 1 1 calc R . . C53 C 0.87564(11) 0.10457(18) 0.87266(13) 0.0395(5) Uani 1 1 d . . . H53A H 0.9218 0.1139 0.8980 0.059 Uiso 1 1 calc R . . H53B H 0.8786 0.0423 0.8355 0.059 Uiso 1 1 calc R . . H53C H 0.8392 0.0869 0.9110 0.059 Uiso 1 1 calc R . . C54 C 0.92054(10) 0.63013(16) 0.87594(11) 0.0279(4) Uani 1 1 d . . . H54A H 0.9097 0.6384 0.8202 0.033 Uiso 1 1 calc R . . C55 C 1.00174(11) 0.62253(18) 0.88453(14) 0.0415(5) Uani 1 1 d . . . H55A H 1.0194 0.5562 0.8563 0.062 Uiso 1 1 calc R . . H55B H 1.0140 0.6148 0.9388 0.062 Uiso 1 1 calc R . . H55C H 1.0236 0.6917 0.8640 0.062 Uiso 1 1 calc R . . C56 C 0.89356(13) 0.73663(18) 0.91639(13) 0.0430(5) Uani 1 1 d . . . H56A H 0.8414 0.7376 0.9153 0.065 Uiso 1 1 calc R . . H56B H 0.9119 0.8043 0.8902 0.065 Uiso 1 1 calc R . . H56C H 0.9100 0.7364 0.9696 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0203(3) 0.0187(2) 0.0248(3) 0.0010(3) -0.0008(3) 0.0009(2) C40 0.0266(10) 0.0228(9) 0.0409(13) -0.0014(11) 0.0000(10) -0.0001(8) C41 0.0280(8) 0.0227(9) 0.0316(10) 0.0014(10) -0.0003(9) -0.0017(8) C42 0.0295(9) 0.0223(9) 0.0212(9) -0.0014(9) 0.0008(8) 0.0019(7) C43 0.0386(11) 0.0285(10) 0.0349(11) 0.0000(10) -0.0004(9) 0.0078(9) N1 0.0195(6) 0.0246(8) 0.0206(7) -0.0004(8) -0.0016(7) -0.0005(6) C10 0.0227(10) 0.0318(10) 0.0208(9) 0.0004(9) -0.0002(8) -0.0024(9) C11 0.0259(11) 0.0426(12) 0.0334(11) 0.0109(11) -0.0076(9) 0.0000(10) C12 0.0229(8) 0.0359(11) 0.0456(12) 0.0057(12) 0.0034(10) 0.0081(8) C13 0.0331(12) 0.0289(11) 0.0340(11) -0.0016(10) 0.0078(9) 0.0037(9) C14 0.0250(11) 0.0247(10) 0.0234(9) 0.0011(9) 0.0035(8) -0.0013(8) C15 0.0360(12) 0.0403(12) 0.0323(11) -0.0146(11) -0.0025(9) -0.0043(10) C16 0.0322(12) 0.0508(14) 0.0217(10) 0.0007(11) -0.0003(8) -0.0048(11) C17 0.0339(12) 0.0326(11) 0.0324(11) 0.0081(10) 0.0034(9) -0.0021(10) C18 0.0365(12) 0.0459(13) 0.0232(10) -0.0007(11) 0.0035(9) -0.0070(11) C1 0.0229(8) 0.0125(7) 0.0164(8) -0.0008(8) -0.0015(7) -0.0037(7) N2 0.0171(7) 0.0160(7) 0.0157(7) 0.0006(7) -0.0001(6) -0.0001(6) N3 0.0211(8) 0.0187(8) 0.0154(7) 0.0013(7) -0.0004(6) -0.0022(6) C2 0.0190(9) 0.0237(9) 0.0236(9) -0.0005(9) 0.0008(7) 0.0006(8) C3 0.0172(8) 0.0244(9) 0.0204(10) 0.0000(9) -0.0022(7) 0.0029(7) C23 0.0179(9) 0.0280(9) 0.0146(8) -0.0001(9) 0.0033(7) 0.0011(8) C24 0.0206(9) 0.0286(10) 0.0215(9) -0.0031(9) 0.0026(8) -0.0006(8) C25 0.0242(9) 0.0398(12) 0.0226(9) -0.0076(10) -0.0036(8) -0.0020(9) C26 0.0335(11) 0.0507(14) 0.0167(9) 0.0028(11) -0.0043(8) 0.0056(10) C27 0.0401(12) 0.0343(11) 0.0248(10) 0.0096(10) -0.0004(9) 0.0044(10) C28 0.0255(10) 0.0281(11) 0.0186(9) 0.0031(9) 0.0039(8) 0.0013(8) C29 0.0388(11) 0.0287(10) 0.0224(9) -0.0027(10) -0.0021(9) -0.0099(9) C30 0.0376(12) 0.0323(12) 0.0655(15) 0.0014(13) -0.0119(11) 0.0006(10) C31 0.0418(12) 0.0371(12) 0.0527(14) -0.0068(13) 0.0096(11) -0.0132(10) C32 0.0405(12) 0.0209(9) 0.0253(9) 0.0012(9) 0.0045(9) -0.0013(9) C33 0.0862(19) 0.0268(11) 0.0356(12) 0.0043(11) 0.0013(13) 0.0103(12) C34 0.0503(13) 0.0377(12) 0.0629(15) -0.0113(14) 0.0119(12) -0.0161(11) C35 0.0188(9) 0.0282(10) 0.0131(8) 0.0031(9) -0.0011(7) 0.0015(8) C36 0.0211(9) 0.0279(10) 0.0225(9) 0.0038(9) -0.0014(8) 0.0023(8) C37 0.0322(11) 0.0385(12) 0.0201(10) 0.0101(10) 0.0043(8) 0.0005(9) C38 0.0357(12) 0.0537(14) 0.0180(9) 0.0052(11) 0.0041(9) 0.0008(11) C39 0.0313(10) 0.0377(12) 0.0211(9) -0.0065(10) -0.0008(8) 0.0039(10) C50 0.0197(9) 0.0320(11) 0.0203(9) -0.0012(9) -0.0048(7) 0.0028(8) C51 0.0343(11) 0.0222(10) 0.0275(10) 0.0056(9) 0.0091(9) -0.0014(8) C52 0.0445(12) 0.0223(10) 0.0368(11) 0.0033(10) -0.0014(10) -0.0031(9) C53 0.0405(12) 0.0304(11) 0.0475(13) 0.0103(11) 0.0079(10) 0.0065(10) C54 0.0357(11) 0.0264(10) 0.0215(9) -0.0051(9) -0.0038(8) -0.0001(9) C55 0.0380(12) 0.0353(11) 0.0512(13) -0.0051(12) -0.0034(10) -0.0089(10) C56 0.0576(14) 0.0339(12) 0.0375(11) -0.0111(11) -0.0055(11) 0.0033(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 N1 1.9802(14) . ? Mg1 C40 2.126(2) . ? Mg1 C1 2.2541(16) . ? C40 C41 1.529(2) . ? C40 H40A 0.92(2) . ? C40 H40B 0.93(3) . ? C41 C42 1.520(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.520(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? N1 C10 1.465(2) . ? N1 C14 1.465(2) . ? C10 C11 1.530(3) . ? C10 C15 1.540(3) . ? C10 C16 1.540(3) . ? C11 C12 1.520(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.524(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.543(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C18 1.523(3) . ? C14 C17 1.553(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C1 N3 1.360(2) . ? C1 N2 1.362(2) . ? N2 C2 1.386(2) . ? N2 C23 1.449(2) . ? N3 C3 1.386(2) . ? N3 C35 1.462(2) . ? C2 C3 1.346(2) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C23 C28 1.395(3) . ? C23 C24 1.404(3) . ? C24 C25 1.403(3) . ? C24 C29 1.510(3) . ? C25 C26 1.376(3) . ? C25 H25A 0.9500 . ? C26 C27 1.375(3) . ? C26 H26A 0.9500 . ? C27 C28 1.392(3) . ? C27 H27A 0.9500 . ? C28 C32 1.512(3) . ? C29 C30 1.531(3) . ? C29 C31 1.532(3) . ? C29 H29A 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C34 1.537(3) . ? C32 C33 1.539(3) . ? C32 H32A 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C50 1.394(3) . ? C35 C36 1.397(3) . ? C36 C37 1.391(3) . ? C36 C51 1.512(3) . ? C37 C38 1.378(3) . ? C37 H37A 0.9500 . ? C38 C39 1.388(3) . ? C38 H38A 0.9500 . ? C39 C50 1.394(3) . ? C39 H39A 0.9500 . ? C50 C54 1.515(3) . ? C51 C53 1.527(3) . ? C51 C52 1.529(3) . ? C51 H51A 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C56 1.524(3) . ? C54 C55 1.536(3) . ? C54 H54A 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mg1 C40 125.87(7) . . ? N1 Mg1 C1 125.35(6) . . ? C40 Mg1 C1 108.77(7) . . ? C41 C40 Mg1 114.65(12) . . ? C41 C40 H40A 108.6(13) . . ? Mg1 C40 H40A 114.3(14) . . ? C41 C40 H40B 110.4(15) . . ? Mg1 C40 H40B 107.0(16) . . ? H40A C40 H40B 101(2) . . ? C42 C41 C40 116.09(14) . . ? C42 C41 H41A 108.3 . . ? C40 C41 H41A 108.3 . . ? C42 C41 H41B 108.3 . . ? C40 C41 H41B 108.3 . . ? H41A C41 H41B 107.4 . . ? C41 C42 C43 114.33(15) . . ? C41 C42 H42A 108.7 . . ? C43 C42 H42A 108.7 . . ? C41 C42 H42B 108.7 . . ? C43 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C10 N1 C14 117.20(12) . . ? C10 N1 Mg1 117.85(11) . . ? C14 N1 Mg1 119.59(11) . . ? N1 C10 C11 111.69(15) . . ? N1 C10 C15 113.73(16) . . ? C11 C10 C15 109.89(16) . . ? N1 C10 C16 105.99(14) . . ? C11 C10 C16 108.49(17) . . ? C15 C10 C16 106.74(16) . . ? C12 C11 C10 112.99(16) . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? C10 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 C13 109.86(14) . . ? C11 C12 H12A 109.7 . . ? C13 C12 H12A 109.7 . . ? C11 C12 H12B 109.7 . . ? C13 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C12 C13 C14 111.84(15) . . ? C12 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? C12 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N1 C14 C18 106.51(15) . . ? N1 C14 C13 111.70(15) . . ? C18 C14 C13 108.65(16) . . ? N1 C14 C17 114.10(15) . . ? C18 C14 C17 106.67(16) . . ? C13 C14 C17 108.94(16) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C1 N2 103.12(12) . . ? N3 C1 Mg1 125.44(11) . . ? N2 C1 Mg1 130.05(12) . . ? C1 N2 C2 111.86(13) . . ? C1 N2 C23 123.74(14) . . ? C2 N2 C23 124.24(14) . . ? C1 N3 C3 112.10(13) . . ? C1 N3 C35 122.67(14) . . ? C3 N3 C35 124.96(14) . . ? C3 C2 N2 106.58(16) . . ? C3 C2 H2A 126.7 . . ? N2 C2 H2A 126.7 . . ? C2 C3 N3 106.35(16) . . ? C2 C3 H3A 126.8 . . ? N3 C3 H3A 126.8 . . ? C28 C23 C24 123.44(16) . . ? C28 C23 N2 119.40(16) . . ? C24 C23 N2 117.17(15) . . ? C25 C24 C23 116.57(18) . . ? C25 C24 C29 120.42(18) . . ? C23 C24 C29 122.97(15) . . ? C26 C25 C24 121.02(19) . . ? C26 C25 H25A 119.5 . . ? C24 C25 H25A 119.5 . . ? C27 C26 C25 120.58(17) . . ? C27 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C26 C27 C28 121.46(19) . . ? C26 C27 H27A 119.3 . . ? C28 C27 H27A 119.3 . . ? C27 C28 C23 116.91(18) . . ? C27 C28 C32 121.00(17) . . ? C23 C28 C32 121.94(15) . . ? C24 C29 C30 110.50(16) . . ? C24 C29 C31 112.69(17) . . ? C30 C29 C31 109.98(17) . . ? C24 C29 H29A 107.8 . . ? C30 C29 H29A 107.8 . . ? C31 C29 H29A 107.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 C34 109.57(16) . . ? C28 C32 C33 113.09(17) . . ? C34 C32 C33 110.64(18) . . ? C28 C32 H32A 107.8 . . ? C34 C32 H32A 107.8 . . ? C33 C32 H32A 107.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C50 C35 C36 124.18(15) . . ? C50 C35 N3 119.06(16) . . ? C36 C35 N3 116.73(16) . . ? C37 C36 C35 116.50(18) . . ? C37 C36 C51 120.75(17) . . ? C35 C36 C51 122.73(15) . . ? C38 C37 C36 121.16(19) . . ? C38 C37 H37A 119.4 . . ? C36 C37 H37A 119.4 . . ? C37 C38 C39 120.74(18) . . ? C37 C38 H38A 119.6 . . ? C39 C38 H38A 119.6 . . ? C38 C39 C50 120.7(2) . . ? C38 C39 H39A 119.7 . . ? C50 C39 H39A 119.7 . . ? C39 C50 C35 116.68(17) . . ? C39 C50 C54 121.25(17) . . ? C35 C50 C54 121.99(15) . . ? C36 C51 C53 113.48(16) . . ? C36 C51 C52 110.26(15) . . ? C53 C51 C52 110.37(16) . . ? C36 C51 H51A 107.5 . . ? C53 C51 H51A 107.5 . . ? C52 C51 H51A 107.5 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C50 C54 C56 114.08(16) . . ? C50 C54 C55 110.03(16) . . ? C56 C54 C55 109.46(17) . . ? C50 C54 H54A 107.7 . . ? C56 C54 H54A 107.7 . . ? C55 C54 H54A 107.7 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Mg1 C40 C41 -21.5(2) . . . . ? C1 Mg1 C40 C41 157.63(15) . . . . ? Mg1 C40 C41 C42 -170.86(14) . . . . ? C40 C41 C42 C43 -171.23(18) . . . . ? C40 Mg1 N1 C10 83.88(15) . . . . ? C1 Mg1 N1 C10 -95.08(13) . . . . ? C40 Mg1 N1 C14 -69.59(16) . . . . ? C1 Mg1 N1 C14 111.46(13) . . . . ? C14 N1 C10 C11 48.5(2) . . . . ? Mg1 N1 C10 C11 -105.63(15) . . . . ? C14 N1 C10 C15 -76.61(19) . . . . ? Mg1 N1 C10 C15 129.29(14) . . . . ? C14 N1 C10 C16 166.44(17) . . . . ? Mg1 N1 C10 C16 12.34(19) . . . . ? N1 C10 C11 C12 -50.4(2) . . . . ? C15 C10 C11 C12 76.8(2) . . . . ? C16 C10 C11 C12 -166.88(16) . . . . ? C10 C11 C12 C13 54.3(2) . . . . ? C11 C12 C13 C14 -54.5(2) . . . . ? C10 N1 C14 C18 -167.74(17) . . . . ? Mg1 N1 C14 C18 -14.11(19) . . . . ? C10 N1 C14 C13 -49.2(2) . . . . ? Mg1 N1 C14 C13 104.39(15) . . . . ? C10 N1 C14 C17 74.9(2) . . . . ? Mg1 N1 C14 C17 -131.51(14) . . . . ? C12 C13 C14 N1 51.5(2) . . . . ? C12 C13 C14 C18 168.69(16) . . . . ? C12 C13 C14 C17 -75.5(2) . . . . ? N1 Mg1 C1 N3 -98.70(15) . . . . ? C40 Mg1 C1 N3 82.20(15) . . . . ? N1 Mg1 C1 N2 97.15(15) . . . . ? C40 Mg1 C1 N2 -81.95(16) . . . . ? N3 C1 N2 C2 -0.11(18) . . . . ? Mg1 C1 N2 C2 166.69(12) . . . . ? N3 C1 N2 C23 175.57(15) . . . . ? Mg1 C1 N2 C23 -17.6(2) . . . . ? N2 C1 N3 C3 -0.15(18) . . . . ? Mg1 C1 N3 C3 -167.76(11) . . . . ? N2 C1 N3 C35 -174.41(15) . . . . ? Mg1 C1 N3 C35 18.0(2) . . . . ? C1 N2 C2 C3 0.3(2) . . . . ? C23 N2 C2 C3 -175.32(15) . . . . ? N2 C2 C3 N3 -0.4(2) . . . . ? C1 N3 C3 C2 0.4(2) . . . . ? C35 N3 C3 C2 174.45(17) . . . . ? C1 N2 C23 C28 88.6(2) . . . . ? C2 N2 C23 C28 -96.2(2) . . . . ? C1 N2 C23 C24 -91.09(19) . . . . ? C2 N2 C23 C24 84.0(2) . . . . ? C28 C23 C24 C25 -0.4(3) . . . . ? N2 C23 C24 C25 179.31(15) . . . . ? C28 C23 C24 C29 177.14(17) . . . . ? N2 C23 C24 C29 -3.2(2) . . . . ? C23 C24 C25 C26 -1.1(3) . . . . ? C29 C24 C25 C26 -178.65(17) . . . . ? C24 C25 C26 C27 1.7(3) . . . . ? C25 C26 C27 C28 -1.0(3) . . . . ? C26 C27 C28 C23 -0.4(3) . . . . ? C26 C27 C28 C32 175.18(18) . . . . ? C24 C23 C28 C27 1.1(3) . . . . ? N2 C23 C28 C27 -178.58(16) . . . . ? C24 C23 C28 C32 -174.45(17) . . . . ? N2 C23 C28 C32 5.9(3) . . . . ? C25 C24 C29 C30 77.7(2) . . . . ? C23 C24 C29 C30 -99.8(2) . . . . ? C25 C24 C29 C31 -45.8(2) . . . . ? C23 C24 C29 C31 136.74(18) . . . . ? C27 C28 C32 C34 -85.3(2) . . . . ? C23 C28 C32 C34 90.1(2) . . . . ? C27 C28 C32 C33 38.6(3) . . . . ? C23 C28 C32 C33 -145.99(18) . . . . ? C1 N3 C35 C50 -89.2(2) . . . . ? C3 N3 C35 C50 97.2(2) . . . . ? C1 N3 C35 C36 89.2(2) . . . . ? C3 N3 C35 C36 -84.3(2) . . . . ? C50 C35 C36 C37 2.6(3) . . . . ? N3 C35 C36 C37 -175.78(15) . . . . ? C50 C35 C36 C51 -179.31(16) . . . . ? N3 C35 C36 C51 2.3(2) . . . . ? C35 C36 C37 C38 -0.2(3) . . . . ? C51 C36 C37 C38 -178.41(17) . . . . ? C36 C37 C38 C39 -1.8(3) . . . . ? C37 C38 C39 C50 1.7(3) . . . . ? C38 C39 C50 C35 0.5(3) . . . . ? C38 C39 C50 C54 -176.30(18) . . . . ? C36 C35 C50 C39 -2.7(3) . . . . ? N3 C35 C50 C39 175.63(16) . . . . ? C36 C35 C50 C54 174.08(17) . . . . ? N3 C35 C50 C54 -7.6(2) . . . . ? C37 C36 C51 C53 -40.8(2) . . . . ? C35 C36 C51 C53 141.20(17) . . . . ? C37 C36 C51 C52 83.6(2) . . . . ? C35 C36 C51 C52 -94.4(2) . . . . ? C39 C50 C54 C56 -27.4(2) . . . . ? C35 C50 C54 C56 155.98(17) . . . . ? C39 C50 C54 C55 96.0(2) . . . . ? C35 C50 C54 C55 -80.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.874 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.259 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.035 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 775963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H63 Mg N3 Si2' _chemical_formula_sum 'C37 H63 Mg N3 Si2' _chemical_formula_weight 630.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.5673(8) _cell_length_b 11.0931(4) _cell_length_c 19.6693(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.065(4) _cell_angle_gamma 90.00 _cell_volume 4000.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7170 _cell_measurement_theta_min 2.4577 _cell_measurement_theta_max 31.0107 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.047 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.96179 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41501 _diffrn_reflns_av_R_equivalents 0.0857 _diffrn_reflns_av_sigmaI/netI 0.1454 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 28.00 _reflns_number_total 9642 _reflns_number_gt 4962 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9642 _refine_ls_number_parameters 411 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1694 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1013 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.26173(5) -0.04386(7) 0.25563(4) 0.0209(2) Uani 1 1 d . . . C1 C 0.23997(13) 0.06024(18) 0.15527(12) 0.0160(5) Uani 1 1 d . . . N1 N 0.17591(11) 0.06667(15) 0.11044(10) 0.0155(5) Uani 1 1 d . . . N2 N 0.29053(11) 0.09170(16) 0.11522(10) 0.0163(5) Uani 1 1 d . . . C2 C 0.18664(14) 0.1003(2) 0.04547(13) 0.0213(6) Uani 1 1 d . . . H2A H 0.1502 0.1102 0.0062 0.026 Uiso 1 1 calc R . . C3 C 0.25878(14) 0.1164(2) 0.04835(13) 0.0221(6) Uani 1 1 d . . . H3A H 0.2832 0.1402 0.0116 0.027 Uiso 1 1 calc R . . C4 C 0.10425(13) 0.0583(2) 0.13038(12) 0.0191(6) Uani 1 1 d . . . C5 C 0.06723(14) -0.0517(2) 0.12369(13) 0.0238(6) Uani 1 1 d . . . C6 C -0.00124(15) -0.0537(3) 0.14435(15) 0.0348(7) Uani 1 1 d . . . H6A H -0.0277 -0.1273 0.1422 0.042 Uiso 1 1 calc R . . C7 C -0.03139(15) 0.0484(3) 0.16781(15) 0.0395(8) Uani 1 1 d . . . H7A H -0.0782 0.0444 0.1815 0.047 Uiso 1 1 calc R . . C8 C 0.00512(16) 0.1555(3) 0.17170(16) 0.0365(8) Uani 1 1 d . . . H8A H -0.0168 0.2252 0.1876 0.044 Uiso 1 1 calc R . . C9 C 0.07402(15) 0.1639(2) 0.15273(14) 0.0257(7) Uani 1 1 d . . . C10 C 0.09816(15) -0.1614(2) 0.09302(15) 0.0309(7) Uani 1 1 d . . . H10A H 0.1523 -0.1519 0.0989 0.037 Uiso 1 1 calc R . . C11 C 0.08164(17) -0.2793(2) 0.12741(18) 0.0494(10) Uani 1 1 d . . . H11A H 0.0957 -0.2720 0.1774 0.074 Uiso 1 1 calc R . . H11B H 0.1093 -0.3450 0.1104 0.074 Uiso 1 1 calc R . . H11C H 0.0293 -0.2967 0.1165 0.074 Uiso 1 1 calc R . . C12 C 0.0692(2) -0.1665(3) 0.01554(17) 0.0556(10) Uani 1 1 d . . . H12A H 0.0843 -0.0938 -0.0067 0.083 Uiso 1 1 calc R . . H12B H 0.0159 -0.1713 0.0083 0.083 Uiso 1 1 calc R . . H12C H 0.0890 -0.2378 -0.0044 0.083 Uiso 1 1 calc R . . C13 C 0.11275(17) 0.2847(2) 0.15381(17) 0.0389(8) Uani 1 1 d . . . H13A H 0.1656 0.2693 0.1524 0.047 Uiso 1 1 calc R . . C14 C 0.1069(2) 0.3585(3) 0.21669(19) 0.0704(12) Uani 1 1 d . . . H14A H 0.1281 0.3137 0.2579 0.106 Uiso 1 1 calc R . . H14B H 0.0555 0.3756 0.2186 0.106 Uiso 1 1 calc R . . H14C H 0.1334 0.4346 0.2146 0.106 Uiso 1 1 calc R . . C15 C 0.0814(2) 0.3579(3) 0.08965(19) 0.0703(12) Uani 1 1 d . . . H15A H 0.1086 0.4334 0.0890 0.105 Uiso 1 1 calc R . . H15B H 0.0299 0.3759 0.0909 0.105 Uiso 1 1 calc R . . H15C H 0.0855 0.3110 0.0482 0.105 Uiso 1 1 calc R . . C16 C 0.36734(14) 0.1126(2) 0.13893(13) 0.0195(6) Uani 1 1 d . . . C17 C 0.38766(15) 0.2261(2) 0.16782(14) 0.0239(6) Uani 1 1 d . . . C18 C 0.46155(16) 0.2451(2) 0.18817(15) 0.0339(7) Uani 1 1 d . . . H18A H 0.4776 0.3201 0.2084 0.041 Uiso 1 1 calc R . . C19 C 0.51246(16) 0.1584(3) 0.17986(15) 0.0385(8) Uani 1 1 d . . . H19A H 0.5628 0.1742 0.1944 0.046 Uiso 1 1 calc R . . C20 C 0.49072(15) 0.0481(3) 0.15044(14) 0.0339(7) Uani 1 1 d . . . H20A H 0.5263 -0.0110 0.1450 0.041 Uiso 1 1 calc R . . C21 C 0.41727(14) 0.0233(2) 0.12883(13) 0.0243(6) Uani 1 1 d . . . C22 C 0.33274(15) 0.3235(2) 0.17691(14) 0.0281(7) Uani 1 1 d . . . H22A H 0.2853 0.3008 0.1483 0.034 Uiso 1 1 calc R . . C23 C 0.32052(18) 0.3300(3) 0.25134(16) 0.0455(9) Uani 1 1 d . . . H23A H 0.3030 0.2518 0.2652 0.068 Uiso 1 1 calc R . . H23B H 0.2841 0.3921 0.2560 0.068 Uiso 1 1 calc R . . H23C H 0.3665 0.3502 0.2809 0.068 Uiso 1 1 calc R . . C24 C 0.35461(18) 0.4480(2) 0.15269(17) 0.0489(9) Uani 1 1 d . . . H24A H 0.3656 0.4418 0.1057 0.073 Uiso 1 1 calc R . . H24B H 0.3979 0.4769 0.1834 0.073 Uiso 1 1 calc R . . H24C H 0.3143 0.5048 0.1535 0.073 Uiso 1 1 calc R . . C25 C 0.39457(15) -0.0944(2) 0.09180(14) 0.0269(7) Uani 1 1 d . . . H25A H 0.3405 -0.1025 0.0884 0.032 Uiso 1 1 calc R . . C26 C 0.41291(18) -0.0898(3) 0.01886(15) 0.0437(8) Uani 1 1 d . . . H26A H 0.3898 -0.0190 -0.0051 0.066 Uiso 1 1 calc R . . H26B H 0.3948 -0.1630 -0.0061 0.066 Uiso 1 1 calc R . . H26C H 0.4659 -0.0845 0.0210 0.066 Uiso 1 1 calc R . . C27 C 0.42987(16) -0.2046(2) 0.12996(16) 0.0398(8) Uani 1 1 d . . . H27A H 0.4182 -0.2059 0.1768 0.060 Uiso 1 1 calc R . . H27B H 0.4829 -0.2006 0.1319 0.060 Uiso 1 1 calc R . . H27C H 0.4112 -0.2780 0.1056 0.060 Uiso 1 1 calc R . . N3 N 0.27374(11) 0.02813(17) 0.34969(10) 0.0222(5) Uani 1 1 d . . . Si1 Si 0.36021(4) 0.04491(6) 0.39193(4) 0.02405(18) Uani 1 1 d . . . C30 C 0.42420(15) 0.0358(2) 0.32791(15) 0.0352(7) Uani 1 1 d . . . H30A H 0.4744 0.0454 0.3516 0.053 Uiso 1 1 calc R . . H30B H 0.4128 0.0999 0.2937 0.053 Uiso 1 1 calc R . . H30C H 0.4190 -0.0428 0.3049 0.053 Uiso 1 1 calc R . . C31 C 0.37553(16) 0.1912(2) 0.44010(15) 0.0357(7) Uani 1 1 d . . . H31A H 0.4275 0.1999 0.4585 0.054 Uiso 1 1 calc R . . H31B H 0.3472 0.1918 0.4781 0.054 Uiso 1 1 calc R . . H31C H 0.3600 0.2583 0.4088 0.054 Uiso 1 1 calc R . . C32 C 0.39058(17) -0.0758(2) 0.45676(15) 0.0424(8) Uani 1 1 d . . . H32A H 0.4391 -0.0560 0.4816 0.064 Uiso 1 1 calc R . . H32B H 0.3925 -0.1533 0.4331 0.064 Uiso 1 1 calc R . . H32C H 0.3560 -0.0814 0.4895 0.064 Uiso 1 1 calc R . . Si2 Si 0.19574(4) 0.03649(7) 0.38431(4) 0.0285(2) Uani 1 1 d . . . C33 C 0.11951(16) -0.0308(3) 0.32244(16) 0.0475(8) Uani 1 1 d . . . H33A H 0.0737 -0.0227 0.3409 0.071 Uiso 1 1 calc R . . H33B H 0.1296 -0.1163 0.3157 0.071 Uiso 1 1 calc R . . H33C H 0.1153 0.0114 0.2782 0.071 Uiso 1 1 calc R . . C34 C 0.16735(18) 0.1949(3) 0.40048(17) 0.0522(9) Uani 1 1 d . . . H34A H 0.1188 0.1941 0.4141 0.078 Uiso 1 1 calc R . . H34B H 0.1660 0.2426 0.3584 0.078 Uiso 1 1 calc R . . H34C H 0.2024 0.2306 0.4374 0.078 Uiso 1 1 calc R . . C35 C 0.19793(19) -0.0437(3) 0.46797(16) 0.0609(10) Uani 1 1 d . . . H35A H 0.1497 -0.0393 0.4821 0.091 Uiso 1 1 calc R . . H35B H 0.2341 -0.0056 0.5031 0.091 Uiso 1 1 calc R . . H35C H 0.2111 -0.1283 0.4626 0.091 Uiso 1 1 calc R . . C40 C 0.26827(19) -0.2318(2) 0.23286(16) 0.0298(7) Uani 1 1 d . . . H40A H 0.2444(17) -0.244(2) 0.1853(17) 0.056(10) Uiso 1 1 d . . . H40B H 0.3190(19) -0.249(3) 0.2328(16) 0.060(11) Uiso 1 1 d . . . C41 C 0.23332(19) -0.3209(2) 0.27807(17) 0.0485(9) Uani 1 1 d . . . H41A H 0.1817 -0.2977 0.2775 0.058 Uiso 1 1 calc R . . H41B H 0.2337 -0.4024 0.2576 0.058 Uiso 1 1 calc R . . C42 C 0.2693(2) -0.3265(3) 0.34913(19) 0.0583(10) Uani 1 1 d . . . H42A H 0.2718 -0.2439 0.3684 0.070 Uiso 1 1 calc R . . H42B H 0.3201 -0.3544 0.3497 0.070 Uiso 1 1 calc R . . C43 C 0.23300(19) -0.4087(3) 0.39629(19) 0.0647(11) Uani 1 1 d . . . H43A H 0.2619 -0.4088 0.4425 0.097 Uiso 1 1 calc R . . H43B H 0.2300 -0.4909 0.3778 0.097 Uiso 1 1 calc R . . H43C H 0.1838 -0.3790 0.3988 0.097 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0231(5) 0.0191(4) 0.0207(5) 0.0013(4) 0.0039(4) -0.0010(4) C1 0.0189(14) 0.0074(12) 0.0219(14) -0.0038(10) 0.0035(11) 0.0001(10) N1 0.0166(12) 0.0120(11) 0.0183(11) -0.0026(8) 0.0043(9) -0.0004(8) N2 0.0149(12) 0.0160(10) 0.0186(12) -0.0009(9) 0.0046(9) -0.0018(9) C2 0.0229(16) 0.0252(14) 0.0153(14) -0.0011(11) 0.0019(11) -0.0001(12) C3 0.0255(17) 0.0240(14) 0.0177(15) 0.0015(11) 0.0062(12) -0.0019(12) C4 0.0142(14) 0.0227(14) 0.0203(14) 0.0062(11) 0.0023(11) 0.0005(11) C5 0.0211(15) 0.0251(14) 0.0235(15) 0.0090(13) -0.0014(11) -0.0015(13) C6 0.0249(17) 0.0343(17) 0.0441(19) 0.0173(15) 0.0017(14) -0.0068(14) C7 0.0221(16) 0.0491(19) 0.050(2) 0.0220(17) 0.0147(14) 0.0072(16) C8 0.0325(19) 0.0363(18) 0.045(2) 0.0093(15) 0.0192(15) 0.0131(15) C9 0.0257(17) 0.0264(15) 0.0263(16) 0.0027(12) 0.0079(13) 0.0021(13) C10 0.0219(16) 0.0219(15) 0.046(2) -0.0001(13) -0.0035(14) -0.0049(12) C11 0.039(2) 0.0257(16) 0.079(3) 0.0099(17) -0.0057(19) -0.0066(15) C12 0.072(3) 0.0393(18) 0.053(2) -0.0100(17) 0.000(2) 0.0034(18) C13 0.0330(19) 0.0257(16) 0.062(2) -0.0145(16) 0.0202(16) 0.0006(14) C14 0.076(3) 0.064(2) 0.069(3) -0.028(2) 0.005(2) -0.007(2) C15 0.117(4) 0.0324(19) 0.067(3) 0.0003(19) 0.033(3) -0.023(2) C16 0.0174(15) 0.0238(14) 0.0180(14) 0.0017(11) 0.0056(11) -0.0052(12) C17 0.0220(16) 0.0246(14) 0.0254(16) -0.0006(12) 0.0047(12) -0.0074(12) C18 0.0296(19) 0.0349(17) 0.0374(19) -0.0062(14) 0.0053(14) -0.0120(14) C19 0.0190(17) 0.055(2) 0.042(2) -0.0077(16) 0.0037(14) -0.0104(15) C20 0.0193(16) 0.0431(17) 0.0407(18) -0.0045(16) 0.0087(13) 0.0030(15) C21 0.0209(15) 0.0287(15) 0.0241(15) 0.0006(12) 0.0055(12) -0.0004(12) C22 0.0254(17) 0.0234(15) 0.0351(18) -0.0078(13) 0.0037(13) -0.0078(12) C23 0.054(2) 0.0343(17) 0.051(2) 0.0008(16) 0.0180(18) 0.0084(16) C24 0.054(2) 0.0376(18) 0.057(2) 0.0119(17) 0.0126(18) 0.0010(17) C25 0.0202(16) 0.0283(15) 0.0323(17) -0.0052(13) 0.0046(13) 0.0057(12) C26 0.055(2) 0.0372(17) 0.039(2) -0.0085(15) 0.0085(17) 0.0069(16) C27 0.036(2) 0.0365(17) 0.048(2) -0.0002(15) 0.0096(16) 0.0036(14) N3 0.0250(13) 0.0215(11) 0.0203(12) -0.0001(10) 0.0046(9) -0.0011(10) Si1 0.0247(4) 0.0225(4) 0.0242(4) -0.0008(3) 0.0015(3) -0.0003(4) C30 0.0266(17) 0.0345(16) 0.0441(19) -0.0018(15) 0.0047(14) 0.0036(14) C31 0.0283(18) 0.0358(16) 0.0419(19) -0.0066(14) 0.0019(15) -0.0017(13) C32 0.044(2) 0.0409(18) 0.0372(19) 0.0071(14) -0.0088(16) 0.0000(15) Si2 0.0255(5) 0.0370(4) 0.0233(4) -0.0055(4) 0.0050(3) -0.0019(4) C33 0.0334(19) 0.059(2) 0.052(2) -0.0178(18) 0.0147(16) -0.0119(16) C34 0.041(2) 0.060(2) 0.055(2) -0.0225(18) 0.0077(18) 0.0073(17) C35 0.051(2) 0.091(3) 0.046(2) 0.014(2) 0.0229(18) 0.007(2) C40 0.035(2) 0.0234(15) 0.0305(19) 0.0033(13) 0.0036(15) 0.0001(14) C41 0.060(2) 0.0300(17) 0.055(2) 0.0050(16) 0.0050(19) 0.0072(16) C42 0.050(2) 0.058(2) 0.064(3) 0.0181(19) 0.000(2) -0.0010(18) C43 0.050(2) 0.079(2) 0.063(3) 0.041(2) 0.003(2) -0.0172(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 N3 1.995(2) . ? Mg1 C40 2.140(3) . ? Mg1 C1 2.268(3) . ? Mg1 Si2 3.1112(13) . ? Mg1 Si1 3.1552(14) . ? C1 N2 1.362(3) . ? C1 N1 1.366(3) . ? N1 C2 1.376(3) . ? N1 C4 1.448(3) . ? N2 C3 1.381(3) . ? N2 C16 1.448(3) . ? C2 C3 1.344(3) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C5 1.397(3) . ? C4 C9 1.400(3) . ? C5 C6 1.395(4) . ? C5 C10 1.511(4) . ? C6 C7 1.375(4) . ? C6 H6A 0.9500 . ? C7 C8 1.363(4) . ? C7 H7A 0.9500 . ? C8 C9 1.391(4) . ? C8 H8A 0.9500 . ? C9 C13 1.519(4) . ? C10 C11 1.526(4) . ? C10 C12 1.535(4) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.502(4) . ? C13 C15 1.536(4) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.392(3) . ? C16 C17 1.408(3) . ? C17 C18 1.383(4) . ? C17 C22 1.516(4) . ? C18 C19 1.376(4) . ? C18 H18A 0.9500 . ? C19 C20 1.386(4) . ? C19 H19A 0.9500 . ? C20 C21 1.391(3) . ? C20 H20A 0.9500 . ? C21 C25 1.522(3) . ? C22 C23 1.518(4) . ? C22 C24 1.537(4) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.527(4) . ? C25 C27 1.527(4) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? N3 Si2 1.697(2) . ? N3 Si1 1.698(2) . ? Si1 C30 1.865(3) . ? Si1 C32 1.874(3) . ? Si1 C31 1.878(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? Si2 C35 1.865(3) . ? Si2 C33 1.871(3) . ? Si2 C34 1.876(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C40 C41 1.540(4) . ? C40 H40A 0.98(3) . ? C40 H40B 0.96(3) . ? C41 C42 1.453(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.531(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Mg1 C40 125.62(11) . . ? N3 Mg1 C1 125.59(9) . . ? C40 Mg1 C1 108.79(11) . . ? N3 Mg1 Si2 29.74(6) . . ? C40 Mg1 Si2 119.47(9) . . ? C1 Mg1 Si2 121.56(7) . . ? N3 Mg1 Si1 28.60(6) . . ? C40 Mg1 Si1 115.95(10) . . ? C1 Mg1 Si1 125.50(7) . . ? Si2 Mg1 Si1 57.94(3) . . ? N2 C1 N1 102.9(2) . . ? N2 C1 Mg1 126.10(17) . . ? N1 C1 Mg1 127.29(17) . . ? C1 N1 C2 112.0(2) . . ? C1 N1 C4 124.4(2) . . ? C2 N1 C4 122.9(2) . . ? C1 N2 C3 111.8(2) . . ? C1 N2 C16 126.0(2) . . ? C3 N2 C16 121.7(2) . . ? C3 C2 N1 106.6(2) . . ? C3 C2 H2A 126.7 . . ? N1 C2 H2A 126.7 . . ? C2 C3 N2 106.7(2) . . ? C2 C3 H3A 126.7 . . ? N2 C3 H3A 126.7 . . ? C5 C4 C9 123.1(2) . . ? C5 C4 N1 119.4(2) . . ? C9 C4 N1 117.5(2) . . ? C6 C5 C4 116.4(2) . . ? C6 C5 C10 121.7(2) . . ? C4 C5 C10 121.9(2) . . ? C7 C6 C5 121.5(3) . . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? C8 C7 C6 120.8(3) . . ? C8 C7 H7A 119.6 . . ? C6 C7 H7A 119.6 . . ? C7 C8 C9 120.9(3) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? C8 C9 C4 117.3(2) . . ? C8 C9 C13 120.6(2) . . ? C4 C9 C13 122.0(2) . . ? C5 C10 C11 113.4(3) . . ? C5 C10 C12 109.3(2) . . ? C11 C10 C12 110.2(2) . . ? C5 C10 H10A 107.9 . . ? C11 C10 H10A 107.9 . . ? C12 C10 H10A 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C9 113.4(3) . . ? C14 C13 C15 108.7(3) . . ? C9 C13 C15 109.7(3) . . ? C14 C13 H13A 108.3 . . ? C9 C13 H13A 108.3 . . ? C15 C13 H13A 108.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 123.5(2) . . ? C21 C16 N2 119.0(2) . . ? C17 C16 N2 117.4(2) . . ? C18 C17 C16 116.4(2) . . ? C18 C17 C22 120.8(2) . . ? C16 C17 C22 122.9(2) . . ? C19 C18 C17 121.8(3) . . ? C19 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? C18 C19 C20 120.4(3) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C20 C21 120.7(3) . . ? C19 C20 H20A 119.7 . . ? C21 C20 H20A 119.7 . . ? C20 C21 C16 117.3(2) . . ? C20 C21 C25 120.1(2) . . ? C16 C21 C25 122.6(2) . . ? C17 C22 C23 110.7(2) . . ? C17 C22 C24 112.9(2) . . ? C23 C22 C24 110.1(2) . . ? C17 C22 H22A 107.7 . . ? C23 C22 H22A 107.7 . . ? C24 C22 H22A 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 109.6(2) . . ? C21 C25 C27 112.7(2) . . ? C26 C25 C27 110.3(2) . . ? C21 C25 H25A 108.0 . . ? C26 C25 H25A 108.0 . . ? C27 C25 H25A 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 N3 Si1 126.77(12) . . ? Si2 N3 Mg1 114.59(11) . . ? Si1 N3 Mg1 117.17(12) . . ? N3 Si1 C30 108.51(12) . . ? N3 Si1 C32 114.50(12) . . ? C30 Si1 C32 105.38(14) . . ? N3 Si1 C31 113.46(12) . . ? C30 Si1 C31 109.00(13) . . ? C32 Si1 C31 105.60(13) . . ? C30 Si1 Mg1 75.81(9) . . ? C32 Si1 Mg1 115.28(9) . . ? C31 Si1 Mg1 136.04(9) . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N3 Si2 C35 115.24(13) . . ? N3 Si2 C33 108.86(12) . . ? C35 Si2 C33 107.02(15) . . ? N3 Si2 C34 113.55(13) . . ? C35 Si2 C34 105.35(16) . . ? C33 Si2 C34 106.27(15) . . ? C35 Si2 Mg1 128.64(11) . . ? C33 Si2 Mg1 73.20(10) . . ? C34 Si2 Mg1 124.29(11) . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C40 Mg1 117.5(2) . . ? C41 C40 H40A 107.3(18) . . ? Mg1 C40 H40A 107.5(17) . . ? C41 C40 H40B 112.1(18) . . ? Mg1 C40 H40B 106.2(18) . . ? H40A C40 H40B 106(3) . . ? C42 C41 C40 114.2(3) . . ? C42 C41 H41A 108.7 . . ? C40 C41 H41A 108.7 . . ? C42 C41 H41B 108.7 . . ? C40 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C41 C42 C43 115.3(3) . . ? C41 C42 H42A 108.4 . . ? C43 C42 H42A 108.4 . . ? C41 C42 H42B 108.4 . . ? C43 C42 H42B 108.4 . . ? H42A C42 H42B 107.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Mg1 C1 N2 99.1(2) . . . . ? C40 Mg1 C1 N2 -80.3(2) . . . . ? Si2 Mg1 C1 N2 134.68(16) . . . . ? Si1 Mg1 C1 N2 63.8(2) . . . . ? N3 Mg1 C1 N1 -106.5(2) . . . . ? C40 Mg1 C1 N1 74.0(2) . . . . ? Si2 Mg1 C1 N1 -70.9(2) . . . . ? Si1 Mg1 C1 N1 -141.83(16) . . . . ? N2 C1 N1 C2 0.2(2) . . . . ? Mg1 C1 N1 C2 -158.81(16) . . . . ? N2 C1 N1 C4 -170.58(18) . . . . ? Mg1 C1 N1 C4 30.4(3) . . . . ? N1 C1 N2 C3 -0.1(2) . . . . ? Mg1 C1 N2 C3 159.29(16) . . . . ? N1 C1 N2 C16 172.67(19) . . . . ? Mg1 C1 N2 C16 -28.0(3) . . . . ? C1 N1 C2 C3 -0.3(3) . . . . ? C4 N1 C2 C3 170.7(2) . . . . ? N1 C2 C3 N2 0.2(3) . . . . ? C1 N2 C3 C2 -0.1(3) . . . . ? C16 N2 C3 C2 -173.2(2) . . . . ? C1 N1 C4 C5 -98.3(3) . . . . ? C2 N1 C4 C5 91.9(3) . . . . ? C1 N1 C4 C9 84.6(3) . . . . ? C2 N1 C4 C9 -85.2(3) . . . . ? C9 C4 C5 C6 -3.5(4) . . . . ? N1 C4 C5 C6 179.5(2) . . . . ? C9 C4 C5 C10 174.0(2) . . . . ? N1 C4 C5 C10 -3.0(4) . . . . ? C4 C5 C6 C7 2.1(4) . . . . ? C10 C5 C6 C7 -175.4(3) . . . . ? C5 C6 C7 C8 -0.1(4) . . . . ? C6 C7 C8 C9 -0.6(5) . . . . ? C7 C8 C9 C4 -0.7(4) . . . . ? C7 C8 C9 C13 176.9(3) . . . . ? C5 C4 C9 C8 2.9(4) . . . . ? N1 C4 C9 C8 179.9(2) . . . . ? C5 C4 C9 C13 -174.7(3) . . . . ? N1 C4 C9 C13 2.3(4) . . . . ? C6 C5 C10 C11 -38.9(4) . . . . ? C4 C5 C10 C11 143.7(2) . . . . ? C6 C5 C10 C12 84.5(3) . . . . ? C4 C5 C10 C12 -93.0(3) . . . . ? C8 C9 C13 C14 43.3(4) . . . . ? C4 C9 C13 C14 -139.2(3) . . . . ? C8 C9 C13 C15 -78.5(4) . . . . ? C4 C9 C13 C15 99.0(3) . . . . ? C1 N2 C16 C21 102.2(3) . . . . ? C3 N2 C16 C21 -85.7(3) . . . . ? C1 N2 C16 C17 -81.2(3) . . . . ? C3 N2 C16 C17 90.9(3) . . . . ? C21 C16 C17 C18 -1.7(4) . . . . ? N2 C16 C17 C18 -178.1(2) . . . . ? C21 C16 C17 C22 178.5(2) . . . . ? N2 C16 C17 C22 2.1(4) . . . . ? C16 C17 C18 C19 0.8(4) . . . . ? C22 C17 C18 C19 -179.4(3) . . . . ? C17 C18 C19 C20 0.0(5) . . . . ? C18 C19 C20 C21 0.0(4) . . . . ? C19 C20 C21 C16 -0.9(4) . . . . ? C19 C20 C21 C25 175.4(3) . . . . ? C17 C16 C21 C20 1.7(4) . . . . ? N2 C16 C21 C20 178.1(2) . . . . ? C17 C16 C21 C25 -174.5(2) . . . . ? N2 C16 C21 C25 1.9(4) . . . . ? C18 C17 C22 C23 -77.4(3) . . . . ? C16 C17 C22 C23 102.4(3) . . . . ? C18 C17 C22 C24 46.5(4) . . . . ? C16 C17 C22 C24 -133.7(3) . . . . ? C20 C21 C25 C26 -72.8(3) . . . . ? C16 C21 C25 C26 103.3(3) . . . . ? C20 C21 C25 C27 50.4(3) . . . . ? C16 C21 C25 C27 -133.5(3) . . . . ? C40 Mg1 N3 Si2 -88.06(17) . . . . ? C1 Mg1 N3 Si2 92.56(14) . . . . ? Si1 Mg1 N3 Si2 -167.1(2) . . . . ? C40 Mg1 N3 Si1 79.07(17) . . . . ? C1 Mg1 N3 Si1 -100.31(14) . . . . ? Si2 Mg1 N3 Si1 167.1(2) . . . . ? Si2 N3 Si1 C30 -176.74(14) . . . . ? Mg1 N3 Si1 C30 17.91(16) . . . . ? Si2 N3 Si1 C32 65.88(19) . . . . ? Mg1 N3 Si1 C32 -99.47(15) . . . . ? Si2 N3 Si1 C31 -55.44(18) . . . . ? Mg1 N3 Si1 C31 139.20(13) . . . . ? Si2 N3 Si1 Mg1 165.4(2) . . . . ? C40 Mg1 Si1 N3 -117.42(16) . . . . ? C1 Mg1 Si1 N3 100.67(14) . . . . ? Si2 Mg1 Si1 N3 -7.49(12) . . . . ? N3 Mg1 Si1 C30 -162.50(15) . . . . ? C40 Mg1 Si1 C30 80.08(14) . . . . ? C1 Mg1 Si1 C30 -61.83(12) . . . . ? Si2 Mg1 Si1 C30 -169.99(9) . . . . ? N3 Mg1 Si1 C32 96.95(17) . . . . ? C40 Mg1 Si1 C32 -20.47(16) . . . . ? C1 Mg1 Si1 C32 -162.38(14) . . . . ? Si2 Mg1 Si1 C32 89.46(12) . . . . ? N3 Mg1 Si1 C31 -59.70(18) . . . . ? C40 Mg1 Si1 C31 -177.12(17) . . . . ? C1 Mg1 Si1 C31 40.97(17) . . . . ? Si2 Mg1 Si1 C31 -67.19(15) . . . . ? Si1 N3 Si2 C35 -43.9(2) . . . . ? Mg1 N3 Si2 C35 121.80(15) . . . . ? Si1 N3 Si2 C33 -164.08(15) . . . . ? Mg1 N3 Si2 C33 1.60(16) . . . . ? Si1 N3 Si2 C34 77.78(18) . . . . ? Mg1 N3 Si2 C34 -116.54(14) . . . . ? Si1 N3 Si2 Mg1 -165.7(2) . . . . ? C40 Mg1 Si2 N3 111.06(16) . . . . ? C1 Mg1 Si2 N3 -107.57(14) . . . . ? Si1 Mg1 Si2 N3 7.23(11) . . . . ? N3 Mg1 Si2 C35 -79.78(19) . . . . ? C40 Mg1 Si2 C35 31.27(19) . . . . ? C1 Mg1 Si2 C35 172.65(16) . . . . ? Si1 Mg1 Si2 C35 -72.55(15) . . . . ? N3 Mg1 Si2 C33 -178.42(16) . . . . ? C40 Mg1 Si2 C33 -67.36(16) . . . . ? C1 Mg1 Si2 C33 74.01(13) . . . . ? Si1 Mg1 Si2 C33 -171.19(11) . . . . ? N3 Mg1 Si2 C34 83.06(17) . . . . ? C40 Mg1 Si2 C34 -165.89(17) . . . . ? C1 Mg1 Si2 C34 -24.51(15) . . . . ? Si1 Mg1 Si2 C34 90.28(13) . . . . ? N3 Mg1 C40 C41 40.1(3) . . . . ? C1 Mg1 C40 C41 -140.4(2) . . . . ? Si2 Mg1 C40 C41 5.4(3) . . . . ? Si1 Mg1 C40 C41 71.6(3) . . . . ? Mg1 C40 C41 C42 -66.9(4) . . . . ? C40 C41 C42 C43 176.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.496 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.049 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 775964' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H63 Al N2' _chemical_formula_sum 'C39 H63 Al N2' _chemical_formula_weight 586.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5150(5) _cell_length_b 10.4747(4) _cell_length_c 19.0528(8) _cell_angle_alpha 97.775(3) _cell_angle_beta 97.597(4) _cell_angle_gamma 93.331(4) _cell_volume 1859.37(14) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3933 _cell_measurement_theta_min 2.8064 _cell_measurement_theta_max 29.6457 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73517 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16290 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.1661 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8474 _reflns_number_gt 4024 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8474 _refine_ls_number_parameters 414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1439 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 0.832 _refine_ls_restrained_S_all 0.832 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.95591(7) 0.83049(5) 0.25290(3) 0.02128(16) Uani 1 1 d . . . C1 C 1.1796(2) 0.86995(16) 0.26804(8) 0.0177(5) Uani 1 1 d . . . N1 N 1.27144(17) 0.83592(14) 0.22076(7) 0.0194(4) Uani 1 1 d . . . N2 N 1.27014(18) 0.91949(14) 0.32912(7) 0.0210(4) Uani 1 1 d . . . C2 C 1.4117(2) 0.86324(18) 0.25088(9) 0.0269(5) Uani 1 1 d . . . H2A H 1.4930 0.8475 0.2279 0.032 Uiso 1 1 calc R . . C3 C 1.4107(2) 0.91633(18) 0.31886(10) 0.0275(5) Uani 1 1 d . . . H3A H 1.4914 0.9461 0.3534 0.033 Uiso 1 1 calc R . . C4 C 1.2305(2) 0.78067(17) 0.14605(8) 0.0187(5) Uani 1 1 d . . . C5 C 1.2201(2) 0.86604(17) 0.09554(9) 0.0229(5) Uani 1 1 d . . . C6 C 1.1813(2) 0.81063(18) 0.02404(9) 0.0260(5) Uani 1 1 d . . . H6A H 1.1734 0.8647 -0.0123 0.031 Uiso 1 1 calc R . . C7 C 1.1544(2) 0.67882(19) 0.00536(9) 0.0265(5) Uani 1 1 d . . . H7A H 1.1267 0.6433 -0.0434 0.032 Uiso 1 1 calc R . . C8 C 1.1674(2) 0.59832(18) 0.05691(9) 0.0241(5) Uani 1 1 d . . . H8A H 1.1486 0.5077 0.0430 0.029 Uiso 1 1 calc R . . C9 C 1.2073(2) 0.64662(18) 0.12869(9) 0.0209(5) Uani 1 1 d . . . C10 C 1.2510(2) 1.01139(18) 0.11545(10) 0.0318(6) Uani 1 1 d . . . H10A H 1.2649 1.0316 0.1688 0.038 Uiso 1 1 calc R . . C11 C 1.1277(3) 1.0848(2) 0.08659(11) 0.0443(7) Uani 1 1 d . . . H11A H 1.0403 1.0531 0.1028 0.066 Uiso 1 1 calc R . . H11B H 1.1159 1.0712 0.0342 0.066 Uiso 1 1 calc R . . H11C H 1.1476 1.1772 0.1043 0.066 Uiso 1 1 calc R . . C12 C 1.3890(3) 1.0551(2) 0.08963(12) 0.0483(7) Uani 1 1 d . . . H12A H 1.4674 1.0098 0.1110 0.072 Uiso 1 1 calc R . . H12B H 1.4092 1.1485 0.1040 0.072 Uiso 1 1 calc R . . H12C H 1.3789 1.0351 0.0374 0.072 Uiso 1 1 calc R . . C13 C 1.2297(2) 0.55546(18) 0.18426(9) 0.0262(5) Uani 1 1 d . . . H13A H 1.2415 0.6081 0.2328 0.031 Uiso 1 1 calc R . . C14 C 1.3657(3) 0.4877(2) 0.17656(11) 0.0479(7) Uani 1 1 d . . . H14A H 1.4472 0.5523 0.1849 0.072 Uiso 1 1 calc R . . H14B H 1.3588 0.4399 0.1282 0.072 Uiso 1 1 calc R . . H14C H 1.3786 0.4276 0.2117 0.072 Uiso 1 1 calc R . . C15 C 1.1043(2) 0.45600(18) 0.17881(10) 0.0373(6) Uani 1 1 d . . . H15A H 1.0176 0.5004 0.1841 0.056 Uiso 1 1 calc R . . H15B H 1.1217 0.4020 0.2168 0.056 Uiso 1 1 calc R . . H15C H 1.0927 0.4015 0.1321 0.056 Uiso 1 1 calc R . . C16 C 1.2292(2) 0.96739(18) 0.39860(9) 0.0194(5) Uani 1 1 d . . . C17 C 1.1839(2) 1.09238(17) 0.40996(9) 0.0213(5) Uani 1 1 d . . . C18 C 1.1556(2) 1.13649(18) 0.47824(9) 0.0242(5) Uani 1 1 d . . . H18A H 1.1226 1.2201 0.4878 0.029 Uiso 1 1 calc R . . C19 C 1.1743(2) 1.06152(19) 0.53255(9) 0.0283(5) Uani 1 1 d . . . H19A H 1.1556 1.0945 0.5791 0.034 Uiso 1 1 calc R . . C20 C 1.2195(2) 0.93983(19) 0.51973(9) 0.0255(5) Uani 1 1 d . . . H20A H 1.2313 0.8894 0.5577 0.031 Uiso 1 1 calc R . . C21 C 1.2486(2) 0.88820(17) 0.45216(9) 0.0205(5) Uani 1 1 d . . . C22 C 1.1695(2) 1.17839(18) 0.35134(9) 0.0259(5) Uani 1 1 d . . . H22A H 1.1309 1.1222 0.3053 0.031 Uiso 1 1 calc R . . C23 C 1.0669(3) 1.28427(18) 0.36386(10) 0.0369(6) Uani 1 1 d . . . H23A H 0.9755 1.2451 0.3720 0.055 Uiso 1 1 calc R . . H23B H 1.0525 1.3288 0.3217 0.055 Uiso 1 1 calc R . . H23C H 1.1072 1.3465 0.4058 0.055 Uiso 1 1 calc R . . C24 C 1.3142(2) 1.2408(2) 0.34233(11) 0.0461(7) Uani 1 1 d . . . H24A H 1.3794 1.1734 0.3333 0.069 Uiso 1 1 calc R . . H24B H 1.3529 1.2993 0.3861 0.069 Uiso 1 1 calc R . . H24C H 1.3028 1.2898 0.3019 0.069 Uiso 1 1 calc R . . C25 C 1.3056(2) 0.75585(18) 0.44158(10) 0.0296(5) Uani 1 1 d . . . H25A H 1.3040 0.7287 0.3891 0.036 Uiso 1 1 calc R . . C26 C 1.2175(3) 0.65267(19) 0.47025(10) 0.0416(7) Uani 1 1 d . . . H26A H 1.1183 0.6490 0.4479 0.062 Uiso 1 1 calc R . . H26B H 1.2227 0.6746 0.5222 0.062 Uiso 1 1 calc R . . H26C H 1.2553 0.5684 0.4590 0.062 Uiso 1 1 calc R . . C27 C 1.4604(2) 0.7633(2) 0.47779(11) 0.0437(6) Uani 1 1 d . . . H27A H 1.5185 0.8242 0.4567 0.066 Uiso 1 1 calc R . . H27B H 1.4968 0.6775 0.4706 0.066 Uiso 1 1 calc R . . H27C H 1.4649 0.7928 0.5291 0.066 Uiso 1 1 calc R . . C30 C 0.8888(2) 0.7620(2) 0.15042(10) 0.0249(5) Uani 1 1 d . . . H30A H 0.931(2) 0.8157(16) 0.1203(9) 0.026(5) Uiso 1 1 d . . . H30B H 0.925(2) 0.6746(18) 0.1379(8) 0.035(6) Uiso 1 1 d . . . C31 C 0.7277(2) 0.74942(18) 0.12755(9) 0.0259(5) Uani 1 1 d . . . H31A H 0.6919 0.8365 0.1340 0.031 Uiso 1 1 calc R . . H31B H 0.6828 0.6973 0.1594 0.031 Uiso 1 1 calc R . . C32 C 0.6818(2) 0.6868(2) 0.04986(10) 0.0346(6) Uani 1 1 d . . . H32A H 0.7330 0.7347 0.0184 0.042 Uiso 1 1 calc R . . H32B H 0.7109 0.5972 0.0445 0.042 Uiso 1 1 calc R . . C33 C 0.5243(2) 0.6833(2) 0.02497(10) 0.0395(6) Uani 1 1 d . . . H33A H 0.5032 0.6405 -0.0247 0.059 Uiso 1 1 calc R . . H33B H 0.4950 0.7718 0.0278 0.059 Uiso 1 1 calc R . . H33C H 0.4724 0.6355 0.0555 0.059 Uiso 1 1 calc R . . C40 C 0.9333(2) 0.7005(2) 0.31848(11) 0.0236(5) Uani 1 1 d . . . H40A H 0.9642(18) 0.7388(15) 0.3671(9) 0.022(5) Uiso 1 1 d . . . H40B H 0.998(2) 0.6313(16) 0.3105(8) 0.022(5) Uiso 1 1 d . . . C41 C 0.7817(2) 0.63759(18) 0.31324(9) 0.0272(5) Uani 1 1 d . . . H41A H 0.7160 0.7071 0.3183 0.033 Uiso 1 1 calc R . . H41B H 0.7551 0.5879 0.2648 0.033 Uiso 1 1 calc R . . C42 C 0.7593(2) 0.54791(19) 0.36801(10) 0.0322(6) Uani 1 1 d . . . H42A H 0.7809 0.5980 0.4166 0.039 Uiso 1 1 calc R . . H42B H 0.8270 0.4799 0.3644 0.039 Uiso 1 1 calc R . . C43 C 0.6082(2) 0.48363(19) 0.35834(10) 0.0386(6) Uani 1 1 d . . . H43A H 0.5970 0.4366 0.3986 0.058 Uiso 1 1 calc R . . H43B H 0.5911 0.4232 0.3136 0.058 Uiso 1 1 calc R . . H43C H 0.5398 0.5499 0.3567 0.058 Uiso 1 1 calc R . . C50 C 0.8533(2) 0.98750(19) 0.27802(10) 0.0230(5) Uani 1 1 d . . . H50A H 0.757(2) 0.9537(17) 0.2815(9) 0.032(6) Uiso 1 1 d . . . H50B H 0.8886(19) 1.0339(15) 0.3263(9) 0.023(5) Uiso 1 1 d . . . C51 C 0.8357(2) 1.08409(18) 0.22413(9) 0.0247(5) Uani 1 1 d . . . H51A H 0.9287 1.1328 0.2257 0.030 Uiso 1 1 calc R . . H51B H 0.8108 1.0346 0.1755 0.030 Uiso 1 1 calc R . . C52 C 0.7247(2) 1.18076(18) 0.23543(9) 0.0297(5) Uani 1 1 d . . . H52A H 0.7476 1.2298 0.2842 0.036 Uiso 1 1 calc R . . H52B H 0.6305 1.1332 0.2320 0.036 Uiso 1 1 calc R . . C53 C 0.7166(2) 1.27576(19) 0.18101(10) 0.0395(6) Uani 1 1 d . . . H53A H 0.6418 1.3340 0.1898 0.059 Uiso 1 1 calc R . . H53B H 0.6947 1.2278 0.1325 0.059 Uiso 1 1 calc R . . H53C H 0.8082 1.3264 0.1859 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0179(4) 0.0252(4) 0.0197(3) 0.0000(2) 0.0026(3) 0.0010(3) C1 0.0218(14) 0.0171(10) 0.0144(10) 0.0011(7) 0.0042(9) 0.0029(9) N1 0.0166(11) 0.0255(9) 0.0153(9) 0.0004(6) 0.0022(7) 0.0002(8) N2 0.0169(11) 0.0302(10) 0.0145(8) -0.0013(7) 0.0027(7) -0.0014(8) C2 0.0140(13) 0.0449(14) 0.0211(11) 0.0007(9) 0.0051(9) 0.0003(11) C3 0.0125(13) 0.0453(14) 0.0217(11) -0.0012(9) 0.0004(9) -0.0046(11) C4 0.0143(13) 0.0277(12) 0.0128(10) -0.0021(8) 0.0027(8) 0.0011(9) C5 0.0209(14) 0.0274(12) 0.0207(11) 0.0029(9) 0.0034(9) 0.0054(10) C6 0.0268(15) 0.0336(13) 0.0194(11) 0.0078(9) 0.0035(9) 0.0064(11) C7 0.0277(15) 0.0361(13) 0.0137(10) -0.0025(9) 0.0017(9) 0.0029(11) C8 0.0249(14) 0.0222(11) 0.0243(11) -0.0039(9) 0.0066(9) 0.0029(10) C9 0.0146(13) 0.0296(12) 0.0191(11) 0.0029(8) 0.0045(8) 0.0031(9) C10 0.0427(18) 0.0277(13) 0.0244(11) 0.0027(9) 0.0036(10) 0.0038(12) C11 0.0467(19) 0.0315(14) 0.0571(15) 0.0061(11) 0.0143(13) 0.0092(12) C12 0.0403(19) 0.0348(14) 0.0678(16) 0.0068(11) 0.0044(13) -0.0044(13) C13 0.0288(15) 0.0286(12) 0.0207(11) 0.0032(9) 0.0025(9) 0.0007(11) C14 0.0354(18) 0.0643(17) 0.0518(15) 0.0354(12) 0.0033(12) 0.0125(14) C15 0.0376(17) 0.0308(13) 0.0453(14) 0.0129(10) 0.0048(11) 0.0041(12) C16 0.0147(13) 0.0269(12) 0.0143(10) -0.0028(8) 0.0025(8) -0.0053(10) C17 0.0169(13) 0.0246(12) 0.0199(11) 0.0015(8) -0.0013(9) -0.0068(10) C18 0.0235(14) 0.0231(12) 0.0239(11) -0.0015(9) 0.0020(9) -0.0008(10) C19 0.0301(15) 0.0353(13) 0.0174(11) -0.0041(9) 0.0070(9) -0.0040(11) C20 0.0252(14) 0.0345(13) 0.0167(11) 0.0054(9) 0.0026(9) -0.0033(11) C21 0.0143(13) 0.0258(12) 0.0196(11) 0.0022(8) -0.0001(8) -0.0049(10) C22 0.0260(15) 0.0274(12) 0.0228(11) 0.0048(9) -0.0008(9) -0.0041(11) C23 0.0464(18) 0.0273(13) 0.0350(12) 0.0054(9) -0.0014(11) 0.0008(12) C24 0.0369(18) 0.0550(16) 0.0481(14) 0.0299(12) -0.0034(12) -0.0123(13) C25 0.0333(16) 0.0297(13) 0.0239(11) 0.0007(9) -0.0012(10) 0.0064(11) C26 0.0462(18) 0.0304(13) 0.0451(14) 0.0110(10) -0.0103(12) 0.0009(12) C27 0.0326(17) 0.0507(15) 0.0477(14) 0.0076(11) 0.0010(12) 0.0106(13) C30 0.0184(14) 0.0269(13) 0.0289(12) 0.0011(10) 0.0034(9) 0.0043(11) C31 0.0214(14) 0.0272(12) 0.0272(11) -0.0009(8) 0.0011(9) 0.0016(10) C32 0.0231(15) 0.0454(14) 0.0308(12) -0.0035(10) -0.0031(10) 0.0020(12) C33 0.0303(16) 0.0518(15) 0.0333(13) -0.0007(10) -0.0005(11) 0.0033(12) C40 0.0177(14) 0.0246(12) 0.0272(12) -0.0010(9) 0.0026(9) 0.0032(11) C41 0.0265(15) 0.0256(12) 0.0288(11) 0.0030(9) 0.0035(9) -0.0011(10) C42 0.0315(16) 0.0313(13) 0.0331(12) 0.0084(9) 0.0015(10) -0.0061(11) C43 0.0361(17) 0.0406(14) 0.0391(13) 0.0086(10) 0.0070(11) -0.0090(12) C50 0.0219(15) 0.0263(12) 0.0198(12) 0.0006(9) 0.0035(9) -0.0014(10) C51 0.0215(14) 0.0294(12) 0.0227(11) 0.0012(9) 0.0032(9) 0.0026(10) C52 0.0292(15) 0.0295(12) 0.0302(12) 0.0023(9) 0.0032(10) 0.0073(11) C53 0.0341(17) 0.0361(14) 0.0502(14) 0.0126(11) 0.0047(11) 0.0075(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 C40 1.990(2) . ? Al1 C30 1.9932(19) . ? Al1 C50 1.996(2) . ? Al1 C1 2.118(2) . ? C1 N1 1.364(2) . ? C1 N2 1.373(2) . ? N1 C2 1.378(2) . ? N1 C4 1.455(2) . ? N2 C3 1.379(2) . ? N2 C16 1.461(2) . ? C2 C3 1.340(2) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C9 1.396(2) . ? C4 C5 1.398(2) . ? C5 C6 1.399(2) . ? C5 C10 1.520(2) . ? C6 C7 1.379(2) . ? C6 H6A 0.9500 . ? C7 C8 1.376(2) . ? C7 H7A 0.9500 . ? C8 C9 1.387(2) . ? C8 H8A 0.9500 . ? C9 C13 1.522(2) . ? C10 C11 1.523(3) . ? C10 C12 1.529(3) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.521(3) . ? C13 C14 1.526(3) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.400(2) . ? C16 C21 1.400(2) . ? C17 C18 1.387(2) . ? C17 C22 1.524(2) . ? C18 C19 1.381(2) . ? C18 H18A 0.9500 . ? C19 C20 1.370(3) . ? C19 H19A 0.9500 . ? C20 C21 1.397(2) . ? C20 H20A 0.9500 . ? C21 C25 1.515(3) . ? C22 C24 1.530(3) . ? C22 C23 1.535(3) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.531(3) . ? C25 C27 1.535(3) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C30 C31 1.530(3) . ? C30 H30A 0.964(17) . ? C30 H30B 1.007(19) . ? C31 C32 1.531(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.507(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C40 C41 1.536(3) . ? C40 H40A 0.959(16) . ? C40 H40B 0.989(18) . ? C41 C42 1.522(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.529(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C50 C51 1.537(3) . ? C50 H50A 0.976(19) . ? C50 H50B 0.986(16) . ? C51 C52 1.521(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.529(2) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C40 Al1 C30 113.38(9) . . ? C40 Al1 C50 112.23(9) . . ? C30 Al1 C50 107.58(9) . . ? C40 Al1 C1 101.59(8) . . ? C30 Al1 C1 109.42(8) . . ? C50 Al1 C1 112.65(8) . . ? N1 C1 N2 102.36(16) . . ? N1 C1 Al1 127.55(12) . . ? N2 C1 Al1 129.59(13) . . ? C1 N1 C2 112.37(15) . . ? C1 N1 C4 125.36(16) . . ? C2 N1 C4 122.24(15) . . ? C1 N2 C3 111.84(15) . . ? C1 N2 C16 126.34(16) . . ? C3 N2 C16 121.80(15) . . ? C3 C2 N1 106.54(18) . . ? C3 C2 H2A 126.7 . . ? N1 C2 H2A 126.7 . . ? C2 C3 N2 106.88(17) . . ? C2 C3 H3A 126.6 . . ? N2 C3 H3A 126.6 . . ? C9 C4 C5 123.86(16) . . ? C9 C4 N1 118.71(16) . . ? C5 C4 N1 117.42(16) . . ? C4 C5 C6 116.39(16) . . ? C4 C5 C10 122.94(16) . . ? C6 C5 C10 120.66(16) . . ? C7 C6 C5 121.11(17) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C8 C7 C6 120.48(17) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C7 C8 C9 121.43(17) . . ? C7 C8 H8A 119.3 . . ? C9 C8 H8A 119.3 . . ? C8 C9 C4 116.71(16) . . ? C8 C9 C13 120.56(17) . . ? C4 C9 C13 122.68(16) . . ? C5 C10 C11 111.82(18) . . ? C5 C10 C12 110.26(18) . . ? C11 C10 C12 111.18(17) . . ? C5 C10 H10A 107.8 . . ? C11 C10 H10A 107.8 . . ? C12 C10 H10A 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C9 112.42(16) . . ? C15 C13 C14 110.08(17) . . ? C9 C13 C14 109.74(17) . . ? C15 C13 H13A 108.2 . . ? C9 C13 H13A 108.2 . . ? C14 C13 H13A 108.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 123.56(16) . . ? C17 C16 N2 118.96(16) . . ? C21 C16 N2 117.28(17) . . ? C18 C17 C16 116.70(17) . . ? C18 C17 C22 120.93(18) . . ? C16 C17 C22 122.35(17) . . ? C19 C18 C17 121.43(19) . . ? C19 C18 H18A 119.3 . . ? C17 C18 H18A 119.3 . . ? C20 C19 C18 120.38(18) . . ? C20 C19 H19A 119.8 . . ? C18 C19 H19A 119.8 . . ? C19 C20 C21 121.50(18) . . ? C19 C20 H20A 119.2 . . ? C21 C20 H20A 119.2 . . ? C20 C21 C16 116.42(18) . . ? C20 C21 C25 119.50(17) . . ? C16 C21 C25 123.99(17) . . ? C17 C22 C24 111.23(17) . . ? C17 C22 C23 113.31(17) . . ? C24 C22 C23 109.18(17) . . ? C17 C22 H22A 107.6 . . ? C24 C22 H22A 107.6 . . ? C23 C22 H22A 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 113.16(18) . . ? C21 C25 C27 109.83(16) . . ? C26 C25 C27 109.38(16) . . ? C21 C25 H25A 108.1 . . ? C26 C25 H25A 108.1 . . ? C27 C25 H25A 108.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C31 C30 Al1 116.18(14) . . ? C31 C30 H30A 108.1(11) . . ? Al1 C30 H30A 109.6(10) . . ? C31 C30 H30B 107.8(11) . . ? Al1 C30 H30B 109.9(10) . . ? H30A C30 H30B 104.5(15) . . ? C30 C31 C32 113.90(17) . . ? C30 C31 H31A 108.8 . . ? C32 C31 H31A 108.8 . . ? C30 C31 H31B 108.8 . . ? C32 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C33 C32 C31 114.37(18) . . ? C33 C32 H32A 108.7 . . ? C31 C32 H32A 108.7 . . ? C33 C32 H32B 108.7 . . ? C31 C32 H32B 108.7 . . ? H32A C32 H32B 107.6 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C41 C40 Al1 114.94(14) . . ? C41 C40 H40A 108.5(10) . . ? Al1 C40 H40A 110.1(9) . . ? C41 C40 H40B 108.5(10) . . ? Al1 C40 H40B 110.6(10) . . ? H40A C40 H40B 103.6(14) . . ? C42 C41 C40 115.67(17) . . ? C42 C41 H41A 108.4 . . ? C40 C41 H41A 108.4 . . ? C42 C41 H41B 108.4 . . ? C40 C41 H41B 108.4 . . ? H41A C41 H41B 107.4 . . ? C41 C42 C43 113.43(17) . . ? C41 C42 H42A 108.9 . . ? C43 C42 H42A 108.9 . . ? C41 C42 H42B 108.9 . . ? C43 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C51 C50 Al1 118.22(14) . . ? C51 C50 H50A 105.7(11) . . ? Al1 C50 H50A 104.4(11) . . ? C51 C50 H50B 109.9(9) . . ? Al1 C50 H50B 112.9(10) . . ? H50A C50 H50B 104.3(14) . . ? C52 C51 C50 116.01(16) . . ? C52 C51 H51A 108.3 . . ? C50 C51 H51A 108.3 . . ? C52 C51 H51B 108.3 . . ? C50 C51 H51B 108.3 . . ? H51A C51 H51B 107.4 . . ? C51 C52 C53 112.81(17) . . ? C51 C52 H52A 109.0 . . ? C53 C52 H52A 109.0 . . ? C51 C52 H52B 109.0 . . ? C53 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C40 Al1 C1 N1 109.60(17) . . . . ? C30 Al1 C1 N1 -10.52(19) . . . . ? C50 Al1 C1 N1 -130.13(16) . . . . ? C40 Al1 C1 N2 -60.86(17) . . . . ? C30 Al1 C1 N2 179.02(16) . . . . ? C50 Al1 C1 N2 59.41(18) . . . . ? N2 C1 N1 C2 -0.16(19) . . . . ? Al1 C1 N1 C2 -172.65(13) . . . . ? N2 C1 N1 C4 -178.31(15) . . . . ? Al1 C1 N1 C4 9.2(3) . . . . ? N1 C1 N2 C3 0.5(2) . . . . ? Al1 C1 N2 C3 172.73(13) . . . . ? N1 C1 N2 C16 -177.74(16) . . . . ? Al1 C1 N2 C16 -5.5(3) . . . . ? C1 N1 C2 C3 -0.2(2) . . . . ? C4 N1 C2 C3 178.02(16) . . . . ? N1 C2 C3 N2 0.5(2) . . . . ? C1 N2 C3 C2 -0.6(2) . . . . ? C16 N2 C3 C2 177.69(17) . . . . ? C1 N1 C4 C9 -88.6(2) . . . . ? C2 N1 C4 C9 93.4(2) . . . . ? C1 N1 C4 C5 92.8(2) . . . . ? C2 N1 C4 C5 -85.2(2) . . . . ? C9 C4 C5 C6 1.2(3) . . . . ? N1 C4 C5 C6 179.67(17) . . . . ? C9 C4 C5 C10 -177.7(2) . . . . ? N1 C4 C5 C10 0.7(3) . . . . ? C4 C5 C6 C7 0.4(3) . . . . ? C10 C5 C6 C7 179.3(2) . . . . ? C5 C6 C7 C8 -1.0(3) . . . . ? C6 C7 C8 C9 0.1(3) . . . . ? C7 C8 C9 C4 1.3(3) . . . . ? C7 C8 C9 C13 -176.3(2) . . . . ? C5 C4 C9 C8 -2.0(3) . . . . ? N1 C4 C9 C8 179.50(17) . . . . ? C5 C4 C9 C13 175.5(2) . . . . ? N1 C4 C9 C13 -3.0(3) . . . . ? C4 C5 C10 C11 -126.2(2) . . . . ? C6 C5 C10 C11 55.0(3) . . . . ? C4 C5 C10 C12 109.6(2) . . . . ? C6 C5 C10 C12 -69.3(3) . . . . ? C8 C9 C13 C15 -51.2(3) . . . . ? C4 C9 C13 C15 131.4(2) . . . . ? C8 C9 C13 C14 71.7(2) . . . . ? C4 C9 C13 C14 -105.8(2) . . . . ? C1 N2 C16 C17 -80.5(2) . . . . ? C3 N2 C16 C17 101.5(2) . . . . ? C1 N2 C16 C21 104.5(2) . . . . ? C3 N2 C16 C21 -73.5(2) . . . . ? C21 C16 C17 C18 -1.0(3) . . . . ? N2 C16 C17 C18 -175.72(16) . . . . ? C21 C16 C17 C22 177.46(18) . . . . ? N2 C16 C17 C22 2.8(3) . . . . ? C16 C17 C18 C19 1.4(3) . . . . ? C22 C17 C18 C19 -177.15(18) . . . . ? C17 C18 C19 C20 -1.1(3) . . . . ? C18 C19 C20 C21 0.3(3) . . . . ? C19 C20 C21 C16 0.0(3) . . . . ? C19 C20 C21 C25 176.89(19) . . . . ? C17 C16 C21 C20 0.4(3) . . . . ? N2 C16 C21 C20 175.12(16) . . . . ? C17 C16 C21 C25 -176.36(18) . . . . ? N2 C16 C21 C25 -1.6(3) . . . . ? C18 C17 C22 C24 99.2(2) . . . . ? C16 C17 C22 C24 -79.2(2) . . . . ? C18 C17 C22 C23 -24.2(2) . . . . ? C16 C17 C22 C23 157.32(18) . . . . ? C20 C21 C25 C26 50.6(2) . . . . ? C16 C21 C25 C26 -132.74(19) . . . . ? C20 C21 C25 C27 -71.9(2) . . . . ? C16 C21 C25 C27 104.7(2) . . . . ? C40 Al1 C30 C31 77.16(18) . . . . ? C50 Al1 C30 C31 -47.55(18) . . . . ? C1 Al1 C30 C31 -170.24(14) . . . . ? Al1 C30 C31 C32 -175.56(14) . . . . ? C30 C31 C32 C33 -175.43(18) . . . . ? C30 Al1 C40 C41 -55.26(19) . . . . ? C50 Al1 C40 C41 66.89(18) . . . . ? C1 Al1 C40 C41 -172.54(15) . . . . ? Al1 C40 C41 C42 -174.19(14) . . . . ? C40 C41 C42 C43 -177.56(18) . . . . ? C40 Al1 C50 C51 -168.07(15) . . . . ? C30 Al1 C50 C51 -42.68(18) . . . . ? C1 Al1 C50 C51 77.99(17) . . . . ? Al1 C50 C51 C52 163.91(14) . . . . ? C50 C51 C52 C53 178.38(17) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.253 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.041 #===END #----------------------------------------------------- #--------COMPOUND 4------------------------------ #--------------------------------------------------- data_sdr918 _database_code_depnum_ccdc_archive 'CCDC 775965' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H144 Mg4 N4' _chemical_formula_weight 1331.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.5342(11) _cell_length_b 13.7504(8) _cell_length_c 17.7758(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.904(6) _cell_angle_gamma 90.00 _cell_volume 4283.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6295 _cell_measurement_theta_min 3.19 _cell_measurement_theta_max 73.51 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.032 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.77490 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21729 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0982 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 64.99 _reflns_number_total 21729 _reflns_number_gt 11576 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Disorder in one Pr group was treated as a split over two sites. The Me groups of this were restrained to have approx equal thermal parameters. Twinning of the sample (180 deg about 1 0 0) was treated during processing and a SHELX HKLF5 formatted file was output. BASF refined to 0.12813. Checkcif reports voids - but no residual e density was detected in these. This data has not been SQUEEZED. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21729 _refine_ls_number_parameters 484 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1175 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1760 _refine_ls_wR_factor_gt 0.1561 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.882 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.78188(4) 1.10216(6) 0.01009(4) 0.0371(2) Uani 1 1 d . . . Mg2 Mg 0.93038(5) 1.04506(6) -0.00278(5) 0.0401(2) Uani 1 1 d . . . N1 N 0.72576(11) 1.31220(14) -0.06495(11) 0.0356(5) Uani 1 1 d . . . N2 N 0.72628(11) 1.32406(14) 0.05544(11) 0.0357(5) Uani 1 1 d . . . C1 C 0.74303(12) 1.26030(16) -0.00071(13) 0.0306(6) Uani 1 1 d . . . C2 C 0.69928(15) 1.40499(18) -0.04838(15) 0.0491(7) Uani 1 1 d . . . H2A H 0.6839 1.4534 -0.0838 0.059 Uiso 1 1 calc R . . C3 C 0.69950(14) 1.41338(18) 0.02649(15) 0.0480(7) Uani 1 1 d . . . H3A H 0.6846 1.4686 0.0545 0.058 Uiso 1 1 calc R . . C4 C 0.72721(14) 1.27609(16) -0.14132(13) 0.0317(6) Uani 1 1 d . A . C5 C 0.66528(14) 1.22210(17) -0.16823(14) 0.0359(6) Uani 1 1 d . . . C6 C 0.66458(15) 1.19558(18) -0.24390(14) 0.0458(7) Uani 1 1 d . . . H6A H 0.6227 1.1598 -0.2649 0.055 Uiso 1 1 calc R . . C7 C 0.72385(16) 1.22080(18) -0.28808(15) 0.0485(7) Uani 1 1 d . . . H7A H 0.7227 1.2019 -0.3395 0.058 Uiso 1 1 calc R . . C8 C 0.78470(16) 1.27271(18) -0.25956(15) 0.0511(8) Uani 1 1 d . A . H8A H 0.8251 1.2892 -0.2915 0.061 Uiso 1 1 calc R . . C9 C 0.78843(15) 1.30192(17) -0.18448(14) 0.0418(7) Uani 1 1 d . . . C10 C 0.59736(15) 1.19880(19) -0.12075(15) 0.0472(7) Uani 1 1 d . . . H10A H 0.6141 1.2064 -0.0667 0.057 Uiso 1 1 calc R . . C11 C 0.56840(15) 1.09535(19) -0.13108(15) 0.0616(9) Uani 1 1 d . . . H11A H 0.5261 1.0839 -0.0975 0.092 Uiso 1 1 calc R . . H11B H 0.6098 1.0495 -0.1190 0.092 Uiso 1 1 calc R . . H11C H 0.5506 1.0859 -0.1834 0.092 Uiso 1 1 calc R . . C12 C 0.53327(15) 1.2729(2) -0.13706(18) 0.0726(10) Uani 1 1 d . . . H12A H 0.5518 1.3385 -0.1249 0.109 Uiso 1 1 calc R . . H12B H 0.4895 1.2576 -0.1062 0.109 Uiso 1 1 calc R . . H12C H 0.5176 1.2698 -0.1904 0.109 Uiso 1 1 calc R . . C16 C 0.72969(14) 1.30684(16) 0.13581(13) 0.0331(6) Uani 1 1 d . . . C17 C 0.66880(15) 1.25826(17) 0.16679(14) 0.0394(7) Uani 1 1 d . . . C18 C 0.66976(17) 1.2517(2) 0.24451(16) 0.0549(8) Uani 1 1 d . . . H18A H 0.6291 1.2192 0.2681 0.066 Uiso 1 1 calc R . . C19 C 0.72756(18) 1.2906(2) 0.28831(16) 0.0576(8) Uani 1 1 d . . . H19A H 0.7266 1.2852 0.3416 0.069 Uiso 1 1 calc R . . C20 C 0.78739(17) 1.3376(2) 0.25523(15) 0.0551(8) Uani 1 1 d . . . H20A H 0.8274 1.3644 0.2861 0.066 Uiso 1 1 calc R . . C21 C 0.79002(15) 1.34649(18) 0.17726(14) 0.0412(7) Uani 1 1 d . . . C22 C 0.60140(16) 1.2190(2) 0.12014(17) 0.0548(8) Uani 1 1 d . . . H22A H 0.6198 1.2038 0.0688 0.066 Uiso 1 1 calc R . . C23 C 0.53969(18) 1.2968(2) 0.1114(2) 0.1079(14) Uani 1 1 d . . . H23A H 0.5595 1.3520 0.0831 0.162 Uiso 1 1 calc R . . H23B H 0.5249 1.3189 0.1613 0.162 Uiso 1 1 calc R . . H23C H 0.4951 1.2696 0.0842 0.162 Uiso 1 1 calc R . . C24 C 0.56770(16) 1.1265(2) 0.15162(16) 0.0727(10) Uani 1 1 d . . . H24A H 0.6084 1.0786 0.1606 0.109 Uiso 1 1 calc R . . H24B H 0.5296 1.1002 0.1155 0.109 Uiso 1 1 calc R . . H24C H 0.5433 1.1411 0.1991 0.109 Uiso 1 1 calc R . . C25 C 0.85537(15) 1.4009(2) 0.14240(15) 0.0527(8) Uani 1 1 d . . . H25A H 0.8540 1.3866 0.0872 0.063 Uiso 1 1 calc R . . C26 C 0.93300(16) 1.3703(2) 0.17491(17) 0.0731(10) Uani 1 1 d . . . H26A H 0.9382 1.2995 0.1712 0.110 Uiso 1 1 calc R . . H26B H 0.9376 1.3900 0.2279 0.110 Uiso 1 1 calc R . . H26C H 0.9732 1.4017 0.1466 0.110 Uiso 1 1 calc R . . C27 C 0.84528(18) 1.5108(2) 0.15258(19) 0.0891(12) Uani 1 1 d . . . H27A H 0.7999 1.5325 0.1237 0.134 Uiso 1 1 calc R . . H27B H 0.8903 1.5447 0.1346 0.134 Uiso 1 1 calc R . . H27C H 0.8392 1.5254 0.2060 0.134 Uiso 1 1 calc R . . C30 C 0.88004(17) 1.1100(2) 0.09921(16) 0.0460(7) Uani 1 1 d . . . C31 C 0.85739(18) 1.0527(3) 0.16791(16) 0.0783(10) Uani 1 1 d . . . H31A H 0.8751 0.9847 0.1629 0.094 Uiso 1 1 calc R . . H31B H 0.8011 1.0517 0.1701 0.094 Uiso 1 1 calc R . . C32 C 0.8915(2) 1.0962(2) 0.24243(19) 0.0882(11) Uani 1 1 d . . . H32A H 0.9478 1.0956 0.2400 0.106 Uiso 1 1 calc R . . H32B H 0.8753 1.1650 0.2458 0.106 Uiso 1 1 calc R . . C33 C 0.8704(2) 1.0468(3) 0.3109(2) 0.1245(15) Uani 1 1 d . . . H33A H 0.8955 1.0784 0.3544 0.187 Uiso 1 1 calc R . . H33B H 0.8865 0.9786 0.3087 0.187 Uiso 1 1 calc R . . H33C H 0.8149 1.0499 0.3156 0.187 Uiso 1 1 calc R . . C40 C 0.69577(16) 0.9959(2) 0.03110(17) 0.0451(7) Uani 1 1 d . . . C41 C 0.70608(13) 0.89401(18) -0.00343(15) 0.0512(7) Uani 1 1 d . . . H41A H 0.7048 0.9007 -0.0589 0.061 Uiso 1 1 calc R . . H41B H 0.7574 0.8697 0.0121 0.061 Uiso 1 1 calc R . . C42 C 0.64817(15) 0.81826(19) 0.01713(15) 0.0556(8) Uani 1 1 d . . . H42A H 0.5972 0.8398 -0.0018 0.067 Uiso 1 1 calc R . . H42B H 0.6466 0.8146 0.0727 0.067 Uiso 1 1 calc R . . C43 C 0.66323(16) 0.71629(19) -0.01345(18) 0.0713(9) Uani 1 1 d . . . H43A H 0.6244 0.6713 0.0043 0.107 Uiso 1 1 calc R . . H43B H 0.7139 0.6943 0.0043 0.107 Uiso 1 1 calc R . . H43C H 0.6611 0.7179 -0.0686 0.107 Uiso 1 1 calc R . . C50 C 0.84829(18) 1.0650(2) -0.09838(17) 0.0434(7) Uani 1 1 d . . . C51 C 0.86782(15) 0.97514(17) -0.14376(14) 0.0458(7) Uani 1 1 d . . . H51A H 0.9223 0.9596 -0.1334 0.055 Uiso 1 1 calc R . . H51B H 0.8375 0.9200 -0.1249 0.055 Uiso 1 1 calc R . . C52 C 0.85469(18) 0.9808(2) -0.22815(17) 0.0664(9) Uani 1 1 d . . . H52A H 0.8015 1.0020 -0.2390 0.080 Uiso 1 1 calc R . . H52B H 0.8605 0.9149 -0.2496 0.080 Uiso 1 1 calc R . . C53 C 0.90894(17) 1.0505(2) -0.26810(16) 0.0738(9) Uani 1 1 d . . . H53A H 0.8976 1.0491 -0.3224 0.111 Uiso 1 1 calc R . . H53B H 0.9619 1.0301 -0.2581 0.111 Uiso 1 1 calc R . . H53C H 0.9019 1.1168 -0.2492 0.111 Uiso 1 1 calc R . . C60 C 1.04266(16) 1.1117(2) -0.03261(17) 0.0441(7) Uani 1 1 d . . . C61 C 1.04027(16) 1.21119(18) 0.00706(16) 0.0585(8) Uani 1 1 d . . . H61A H 0.9880 1.2378 0.0005 0.070 Uiso 1 1 calc R . . H61B H 1.0500 1.2007 0.0616 0.070 Uiso 1 1 calc R . . C62 C 1.09579(19) 1.2866(2) -0.0194(2) 0.0872(11) Uani 1 1 d . . . H62A H 1.0858 1.2981 -0.0739 0.105 Uiso 1 1 calc R . . H62B H 1.1482 1.2604 -0.0131 0.105 Uiso 1 1 calc R . . C63 C 1.0919(2) 1.3844(2) 0.0220(2) 0.1216(15) Uani 1 1 d . . . H63A H 1.1318 1.4278 0.0040 0.182 Uiso 1 1 calc R . . H63B H 1.0997 1.3738 0.0762 0.182 Uiso 1 1 calc R . . H63C H 1.0418 1.4141 0.0121 0.182 Uiso 1 1 calc R . . C13 C 0.8426(11) 1.3834(14) -0.1588(12) 0.038(5) Uiso 0.259(6) 1 d P A 1 H13 H 0.8137 1.4314 -0.1285 0.045 Uiso 0.259(6) 1 calc PR A 1 C14 C 0.8832(7) 1.4376(10) -0.2209(7) 0.059(4) Uiso 0.259(6) 1 d PU A 1 H14A H 0.9156 1.4886 -0.1984 0.089 Uiso 0.259(6) 1 calc PR A 1 H14B H 0.8453 1.4670 -0.2556 0.089 Uiso 0.259(6) 1 calc PR A 1 H14C H 0.9148 1.3918 -0.2484 0.089 Uiso 0.259(6) 1 calc PR A 1 C15 C 0.9033(7) 1.3319(8) -0.1062(7) 0.050(4) Uiso 0.259(6) 1 d PU A 1 H15A H 0.9284 1.2802 -0.1342 0.074 Uiso 0.259(6) 1 calc PR A 1 H15B H 0.8782 1.3038 -0.0629 0.074 Uiso 0.259(6) 1 calc PR A 1 H15C H 0.9415 1.3795 -0.0886 0.074 Uiso 0.259(6) 1 calc PR A 1 C15A C 0.9354(2) 1.3171(3) -0.1733(3) 0.0775(18) Uani 0.741(6) 1 d PU A 2 H15D H 0.9403 1.2494 -0.1565 0.116 Uiso 0.741(6) 1 calc PR A 2 H15E H 0.9762 1.3561 -0.1495 0.116 Uiso 0.741(6) 1 calc PR A 2 H15F H 0.9393 1.3199 -0.2281 0.116 Uiso 0.741(6) 1 calc PR A 2 C14A C 0.8523(3) 1.4627(3) -0.1767(4) 0.100(2) Uani 0.741(6) 1 d PU A 2 H14D H 0.8999 1.4967 -0.1630 0.150 Uiso 0.741(6) 1 calc PR A 2 H14E H 0.8097 1.4942 -0.1521 0.150 Uiso 0.741(6) 1 calc PR A 2 H14F H 0.8437 1.4650 -0.2314 0.150 Uiso 0.741(6) 1 calc PR A 2 C13A C 0.8581(4) 1.3571(5) -0.1512(4) 0.0514(17) Uani 0.741(6) 1 d P A 2 H13A H 0.8558 1.3555 -0.0951 0.062 Uiso 0.741(6) 1 calc PR A 2 H30A H 0.9360(14) 1.1193(16) 0.1048(12) 0.053(8) Uiso 1 1 d . . . H30B H 0.8656(15) 1.174(2) 0.1018(15) 0.080(11) Uiso 1 1 d . . . H40A H 0.6452(12) 1.0159(14) 0.0164(11) 0.032(7) Uiso 1 1 d . . . H40B H 0.6910(12) 0.9898(15) 0.0858(13) 0.045(8) Uiso 1 1 d . . . H50A H 0.8718(12) 1.1163(16) -0.1199(12) 0.037(7) Uiso 1 1 d . . . H50B H 0.8016(13) 1.0740(16) -0.1105(12) 0.041(8) Uiso 1 1 d . . . H60A H 1.0942(11) 1.0985(14) -0.0377(10) 0.021(6) Uiso 1 1 d . . . H60B H 1.0320(12) 1.1197(16) -0.0861(13) 0.052(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0371(5) 0.0392(5) 0.0349(5) -0.0004(4) -0.0001(4) 0.0013(4) Mg2 0.0378(5) 0.0392(5) 0.0434(6) -0.0004(4) 0.0016(4) 0.0011(4) N1 0.0397(13) 0.0373(12) 0.0296(12) 0.0022(10) -0.0002(10) -0.0049(10) N2 0.0401(13) 0.0405(12) 0.0263(12) -0.0062(10) -0.0010(10) -0.0028(10) C1 0.0294(14) 0.0374(14) 0.0249(14) -0.0016(12) -0.0019(11) -0.0045(11) C2 0.074(2) 0.0351(15) 0.0374(17) 0.0035(14) -0.0042(15) 0.0090(14) C3 0.070(2) 0.0323(15) 0.0410(17) -0.0049(13) -0.0030(15) 0.0117(14) C4 0.0365(15) 0.0347(14) 0.0238(14) -0.0015(11) 0.0005(11) 0.0018(12) C5 0.0416(16) 0.0354(14) 0.0307(15) 0.0000(12) -0.0007(12) 0.0016(12) C6 0.0539(19) 0.0465(17) 0.0367(17) -0.0023(14) -0.0046(14) -0.0041(14) C7 0.067(2) 0.0484(17) 0.0302(16) -0.0059(13) 0.0005(15) 0.0045(15) C8 0.065(2) 0.0496(18) 0.0391(18) 0.0075(14) 0.0150(15) 0.0018(16) C9 0.0477(18) 0.0412(16) 0.0365(16) 0.0021(13) 0.0023(13) 0.0004(13) C10 0.0436(18) 0.0573(19) 0.0405(17) -0.0064(15) -0.0016(13) -0.0091(15) C11 0.060(2) 0.066(2) 0.058(2) 0.0075(17) -0.0075(16) -0.0251(17) C12 0.045(2) 0.070(2) 0.103(3) 0.007(2) 0.0124(18) 0.0026(17) C16 0.0396(16) 0.0328(14) 0.0271(14) -0.0029(12) 0.0008(12) 0.0061(12) C17 0.0470(17) 0.0357(15) 0.0361(16) -0.0017(13) 0.0104(13) 0.0051(13) C18 0.067(2) 0.0494(17) 0.049(2) -0.0014(15) 0.0173(17) -0.0013(15) C19 0.077(2) 0.065(2) 0.0311(17) -0.0009(15) 0.0092(16) 0.0062(18) C20 0.073(2) 0.0587(19) 0.0330(17) -0.0069(15) -0.0088(16) -0.0029(17) C21 0.0487(18) 0.0426(16) 0.0321(16) -0.0033(13) -0.0006(13) 0.0018(13) C22 0.0453(19) 0.0574(19) 0.062(2) -0.0057(16) 0.0108(16) -0.0086(16) C23 0.056(2) 0.098(3) 0.169(4) 0.002(3) -0.019(2) -0.005(2) C24 0.067(2) 0.074(2) 0.079(2) -0.0152(19) 0.0359(18) -0.0268(18) C25 0.0507(19) 0.0635(19) 0.0433(17) -0.0067(16) -0.0092(14) -0.0169(16) C26 0.060(2) 0.088(2) 0.070(2) -0.0140(19) -0.0094(18) -0.0180(19) C27 0.086(3) 0.051(2) 0.131(3) 0.006(2) 0.006(2) -0.0239(19) C30 0.0378(18) 0.0556(19) 0.0444(18) -0.0001(16) -0.0019(14) 0.0047(16) C31 0.069(2) 0.122(3) 0.043(2) -0.008(2) -0.0096(17) -0.009(2) C32 0.105(3) 0.084(3) 0.076(3) 0.015(2) -0.003(2) 0.009(2) C33 0.162(4) 0.136(4) 0.077(3) 0.019(3) 0.019(3) -0.034(3) C40 0.0418(19) 0.0534(18) 0.0404(19) 0.0005(15) 0.0043(15) 0.0006(14) C41 0.0423(17) 0.0515(17) 0.0601(19) -0.0017(16) 0.0049(14) -0.0042(14) C42 0.057(2) 0.0567(18) 0.0532(19) -0.0007(16) -0.0002(15) -0.0046(15) C43 0.061(2) 0.057(2) 0.095(3) 0.0011(19) 0.0018(19) -0.0028(17) C50 0.0347(19) 0.0446(18) 0.0510(19) 0.0015(15) 0.0025(15) 0.0045(15) C51 0.0525(18) 0.0437(16) 0.0414(17) -0.0062(14) 0.0052(14) -0.0046(14) C52 0.081(2) 0.0537(19) 0.065(2) -0.0100(17) 0.0094(18) -0.0115(17) C53 0.086(2) 0.076(2) 0.059(2) -0.0018(18) 0.0090(18) -0.005(2) C60 0.0360(17) 0.0455(16) 0.051(2) -0.0013(16) 0.0034(15) 0.0044(14) C61 0.072(2) 0.0402(16) 0.064(2) 0.0101(15) 0.0019(17) -0.0058(16) C62 0.096(3) 0.061(2) 0.104(3) 0.009(2) 0.002(2) -0.003(2) C63 0.172(4) 0.056(2) 0.137(4) -0.007(3) 0.018(3) -0.028(3) C15A 0.046(3) 0.089(4) 0.099(4) 0.029(3) 0.008(3) -0.010(2) C14A 0.082(4) 0.048(3) 0.167(7) 0.007(4) -0.039(4) -0.019(3) C13A 0.051(4) 0.054(4) 0.049(3) 0.010(3) 0.004(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 C40 2.143(3) . ? Mg1 C1 2.285(2) . ? Mg1 C30 2.303(3) . ? Mg1 C50 2.342(3) . ? Mg1 Mg2 2.7364(11) . ? Mg1 H30B 2.37(3) . ? Mg1 H50B 2.22(2) . ? Mg2 C50 2.207(3) . ? Mg2 C30 2.229(3) . ? Mg2 C60 2.251(3) . ? Mg2 C60 2.291(3) 3_775 ? Mg2 Mg2 2.7369(16) 3_775 ? Mg2 C51 2.868(3) . ? Mg2 H30A 2.17(2) . ? N1 C1 1.372(3) . ? N1 C2 1.393(3) . ? N1 C4 1.446(3) . ? N2 C1 1.368(3) . ? N2 C3 1.406(3) . ? N2 C16 1.447(3) . ? C2 C3 1.336(3) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C9 1.386(3) . ? C4 C5 1.387(3) . ? C5 C6 1.393(3) . ? C5 C10 1.517(3) . ? C6 C7 1.368(3) . ? C6 H6A 0.9500 . ? C7 C8 1.367(3) . ? C7 H7A 0.9500 . ? C8 C9 1.393(3) . ? C8 H8A 0.9500 . ? C9 C13 1.53(2) . ? C9 C13A 1.540(7) . ? C10 C11 1.519(3) . ? C10 C12 1.537(3) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C16 C21 1.381(3) . ? C16 C17 1.389(3) . ? C17 C18 1.384(3) . ? C17 C22 1.520(3) . ? C18 C19 1.366(4) . ? C18 H18A 0.9500 . ? C19 C20 1.381(3) . ? C19 H19A 0.9500 . ? C20 C21 1.394(3) . ? C20 H20A 0.9500 . ? C21 C25 1.518(3) . ? C22 C24 1.517(3) . ? C22 C23 1.526(4) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.520(3) . ? C25 C27 1.532(3) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C30 C31 1.517(4) . ? C30 H30A 0.99(2) . ? C30 H30B 0.92(3) . ? C31 C32 1.555(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.452(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C40 C41 1.543(3) . ? C40 H40A 0.96(2) . ? C40 H40B 0.98(2) . ? C41 C42 1.508(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.530(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C50 C51 1.521(3) . ? C50 H50A 0.91(2) . ? C50 H50B 0.85(2) . ? C51 C52 1.512(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.540(3) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C60 C61 1.540(3) . ? C60 Mg2 2.291(3) 3_775 ? C60 H60A 0.929(18) . ? C60 H60B 0.97(2) . ? C61 C62 1.509(3) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.535(4) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C13 C14 1.53(2) . ? C13 C15 1.563(19) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C15A C13A 1.526(7) . ? C15A H15D 0.9800 . ? C15A H15E 0.9800 . ? C15A H15F 0.9800 . ? C14A C13A 1.523(7) . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C13A H13A 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C40 Mg1 C1 116.98(10) . . ? C40 Mg1 C30 115.27(12) . . ? C1 Mg1 C30 103.14(10) . . ? C40 Mg1 C50 111.56(11) . . ? C1 Mg1 C50 107.05(9) . . ? C30 Mg1 C50 101.30(11) . . ? C40 Mg1 Mg2 119.80(9) . . ? C1 Mg1 Mg2 123.23(6) . . ? C30 Mg1 Mg2 51.64(8) . . ? C50 Mg1 Mg2 50.81(8) . . ? C40 Mg1 H30B 126.0(7) . . ? C1 Mg1 H30B 80.6(7) . . ? C30 Mg1 H30B 22.6(7) . . ? C50 Mg1 H30B 110.1(7) . . ? Mg2 Mg1 H30B 67.0(7) . . ? C40 Mg1 H50B 100.5(6) . . ? C1 Mg1 H50B 98.1(6) . . ? C30 Mg1 H50B 122.4(6) . . ? C50 Mg1 H50B 21.2(6) . . ? Mg2 Mg1 H50B 71.9(6) . . ? H30B Mg1 H50B 128.6(9) . . ? C50 Mg2 C30 108.09(11) . . ? C50 Mg2 C60 108.72(12) . . ? C30 Mg2 C60 113.67(11) . . ? C50 Mg2 C60 116.87(11) . 3_775 ? C30 Mg2 C60 103.73(11) . 3_775 ? C60 Mg2 C60 105.89(9) . 3_775 ? C50 Mg2 Mg1 55.30(8) . . ? C30 Mg2 Mg1 54.09(8) . . ? C60 Mg2 Mg1 138.15(8) . . ? C60 Mg2 Mg1 115.81(8) 3_775 . ? C50 Mg2 Mg2 129.96(9) . 3_775 ? C30 Mg2 Mg2 121.93(9) . 3_775 ? C60 Mg2 Mg2 53.61(8) . 3_775 ? C60 Mg2 Mg2 52.28(7) 3_775 3_775 ? Mg1 Mg2 Mg2 167.71(5) . 3_775 ? C50 Mg2 C51 31.61(8) . . ? C30 Mg2 C51 134.00(10) . . ? C60 Mg2 C51 104.05(10) . . ? C60 Mg2 C51 89.65(9) 3_775 . ? Mg1 Mg2 C51 80.32(6) . . ? Mg2 Mg2 C51 101.22(7) 3_775 . ? C50 Mg2 H30A 129.1(6) . . ? C30 Mg2 H30A 26.0(6) . . ? C60 Mg2 H30A 90.1(6) . . ? C60 Mg2 H30A 101.4(6) 3_775 . ? Mg1 Mg2 H30A 78.9(6) . . ? Mg2 Mg2 H30A 99.6(6) 3_775 . ? C51 Mg2 H30A 159.1(6) . . ? C1 N1 C2 111.50(19) . . ? C1 N1 C4 126.32(19) . . ? C2 N1 C4 122.0(2) . . ? C1 N2 C3 111.7(2) . . ? C1 N2 C16 127.8(2) . . ? C3 N2 C16 120.4(2) . . ? N2 C1 N1 103.13(19) . . ? N2 C1 Mg1 128.27(17) . . ? N1 C1 Mg1 128.46(16) . . ? C3 C2 N1 107.5(2) . . ? C3 C2 H2A 126.3 . . ? N1 C2 H2A 126.3 . . ? C2 C3 N2 106.2(2) . . ? C2 C3 H3A 126.9 . . ? N2 C3 H3A 126.9 . . ? C9 C4 C5 123.9(2) . . ? C9 C4 N1 118.0(2) . . ? C5 C4 N1 118.0(2) . . ? C4 C5 C6 117.0(2) . . ? C4 C5 C10 122.8(2) . . ? C6 C5 C10 120.0(2) . . ? C7 C6 C5 120.4(2) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C8 C7 C6 121.2(3) . . ? C8 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? C7 C8 C9 121.1(3) . . ? C7 C8 H8A 119.4 . . ? C9 C8 H8A 119.4 . . ? C4 C9 C8 116.3(2) . . ? C4 C9 C13 120.4(9) . . ? C8 C9 C13 120.5(9) . . ? C4 C9 C13A 122.2(3) . . ? C8 C9 C13A 121.5(3) . . ? C5 C10 C11 113.3(2) . . ? C5 C10 C12 109.7(2) . . ? C11 C10 C12 111.0(2) . . ? C5 C10 H10A 107.5 . . ? C11 C10 H10A 107.5 . . ? C12 C10 H10A 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C21 C16 C17 124.3(2) . . ? C21 C16 N2 117.9(2) . . ? C17 C16 N2 117.6(2) . . ? C18 C17 C16 116.3(3) . . ? C18 C17 C22 120.3(3) . . ? C16 C17 C22 123.3(2) . . ? C19 C18 C17 121.8(3) . . ? C19 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? C18 C19 C20 120.0(3) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C19 C20 C21 121.0(3) . . ? C19 C20 H20A 119.5 . . ? C21 C20 H20A 119.5 . . ? C16 C21 C20 116.5(2) . . ? C16 C21 C25 123.5(2) . . ? C20 C21 C25 120.0(2) . . ? C24 C22 C17 113.7(2) . . ? C24 C22 C23 110.0(3) . . ? C17 C22 C23 110.0(2) . . ? C24 C22 H22A 107.6 . . ? C17 C22 H22A 107.6 . . ? C23 C22 H22A 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 112.8(2) . . ? C21 C25 C27 110.2(2) . . ? C26 C25 C27 109.5(2) . . ? C21 C25 H25A 108.1 . . ? C26 C25 H25A 108.1 . . ? C27 C25 H25A 108.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C31 C30 Mg2 124.6(2) . . ? C31 C30 Mg1 108.64(19) . . ? Mg2 C30 Mg1 74.27(9) . . ? C31 C30 H30A 105.7(13) . . ? Mg2 C30 H30A 73.5(13) . . ? Mg1 C30 H30A 142.2(13) . . ? C31 C30 H30B 112.2(18) . . ? Mg2 C30 H30B 122.9(18) . . ? Mg1 C30 H30B 83.1(17) . . ? H30A C30 H30B 98(2) . . ? C30 C31 C32 112.5(3) . . ? C30 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? C30 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C33 C32 C31 115.6(3) . . ? C33 C32 H32A 108.4 . . ? C31 C32 H32A 108.4 . . ? C33 C32 H32B 108.4 . . ? C31 C32 H32B 108.4 . . ? H32A C32 H32B 107.4 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C41 C40 Mg1 117.21(18) . . ? C41 C40 H40A 105.8(13) . . ? Mg1 C40 H40A 114.2(12) . . ? C41 C40 H40B 109.3(13) . . ? Mg1 C40 H40B 108.3(13) . . ? H40A C40 H40B 100.8(17) . . ? C42 C41 C40 116.2(2) . . ? C42 C41 H41A 108.2 . . ? C40 C41 H41A 108.2 . . ? C42 C41 H41B 108.2 . . ? C40 C41 H41B 108.2 . . ? H41A C41 H41B 107.4 . . ? C41 C42 C43 114.9(2) . . ? C41 C42 H42A 108.5 . . ? C43 C42 H42A 108.5 . . ? C41 C42 H42B 108.5 . . ? C43 C42 H42B 108.5 . . ? H42A C42 H42B 107.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C51 C50 Mg2 98.89(18) . . ? C51 C50 Mg1 137.8(2) . . ? Mg2 C50 Mg1 73.89(9) . . ? C51 C50 H50A 107.1(14) . . ? Mg2 C50 H50A 97.3(14) . . ? Mg1 C50 H50A 115.0(14) . . ? C51 C50 H50B 102.4(16) . . ? Mg2 C50 H50B 144.3(16) . . ? Mg1 C50 H50B 71.1(15) . . ? H50A C50 H50B 103(2) . . ? C52 C51 C50 117.0(2) . . ? C52 C51 Mg2 152.96(18) . . ? C50 C51 Mg2 49.50(14) . . ? C52 C51 H51A 108.0 . . ? C50 C51 H51A 108.0 . . ? Mg2 C51 H51A 64.6 . . ? C52 C51 H51B 108.0 . . ? C50 C51 H51B 108.0 . . ? Mg2 C51 H51B 98.9 . . ? H51A C51 H51B 107.3 . . ? C51 C52 C53 114.4(2) . . ? C51 C52 H52A 108.7 . . ? C53 C52 H52A 108.7 . . ? C51 C52 H52B 108.7 . . ? C53 C52 H52B 108.7 . . ? H52A C52 H52B 107.6 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C61 C60 Mg2 102.51(17) . . ? C61 C60 Mg2 135.9(2) . 3_775 ? Mg2 C60 Mg2 74.11(9) . 3_775 ? C61 C60 H60A 105.0(12) . . ? Mg2 C60 H60A 143.5(12) . . ? Mg2 C60 H60A 69.5(12) 3_775 . ? C61 C60 H60B 109.9(14) . . ? Mg2 C60 H60B 97.8(14) . . ? Mg2 C60 H60B 114.1(14) 3_775 . ? H60A C60 H60B 94.8(17) . . ? C62 C61 C60 116.1(2) . . ? C62 C61 H61A 108.3 . . ? C60 C61 H61A 108.3 . . ? C62 C61 H61B 108.3 . . ? C60 C61 H61B 108.3 . . ? H61A C61 H61B 107.4 . . ? C61 C62 C63 114.4(3) . . ? C61 C62 H62A 108.7 . . ? C63 C62 H62A 108.7 . . ? C61 C62 H62B 108.7 . . ? C63 C62 H62B 108.7 . . ? H62A C62 H62B 107.6 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C14 C13 C9 116.2(15) . . ? C14 C13 C15 109.1(14) . . ? C9 C13 C15 104.5(12) . . ? C14 C13 H13 108.9 . . ? C9 C13 H13 108.9 . . ? C15 C13 H13 108.9 . . ? C13A C15A H15D 109.5 . . ? C13A C15A H15E 109.5 . . ? H15D C15A H15E 109.5 . . ? C13A C15A H15F 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? C13A C14A H14D 109.5 . . ? C13A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C13A C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C14A C13A C15A 108.6(5) . . ? C14A C13A C9 108.1(5) . . ? C15A C13A C9 115.0(5) . . ? C14A C13A H13A 108.3 . . ? C15A C13A H13A 108.3 . . ? C9 C13A H13A 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C40 Mg1 Mg2 C50 94.56(14) . . . . ? C1 Mg1 Mg2 C50 -85.31(12) . . . . ? C30 Mg1 Mg2 C50 -165.41(14) . . . . ? C40 Mg1 Mg2 C30 -100.03(14) . . . . ? C1 Mg1 Mg2 C30 80.10(13) . . . . ? C50 Mg1 Mg2 C30 165.41(14) . . . . ? C40 Mg1 Mg2 C60 173.72(16) . . . . ? C1 Mg1 Mg2 C60 -6.14(16) . . . . ? C30 Mg1 Mg2 C60 -86.24(16) . . . . ? C50 Mg1 Mg2 C60 79.16(16) . . . . ? C40 Mg1 Mg2 C60 -11.45(14) . . . 3_775 ? C1 Mg1 Mg2 C60 168.69(11) . . . 3_775 ? C30 Mg1 Mg2 C60 88.59(13) . . . 3_775 ? C50 Mg1 Mg2 C60 -106.00(13) . . . 3_775 ? C40 Mg1 Mg2 Mg2 -24.9(3) . . . 3_775 ? C1 Mg1 Mg2 Mg2 155.3(2) . . . 3_775 ? C30 Mg1 Mg2 Mg2 75.2(3) . . . 3_775 ? C50 Mg1 Mg2 Mg2 -119.4(3) . . . 3_775 ? C40 Mg1 Mg2 C51 73.43(11) . . . . ? C1 Mg1 Mg2 C51 -106.44(9) . . . . ? C30 Mg1 Mg2 C51 173.46(12) . . . . ? C50 Mg1 Mg2 C51 -21.13(11) . . . . ? C3 N2 C1 N1 -0.2(2) . . . . ? C16 N2 C1 N1 176.5(2) . . . . ? C3 N2 C1 Mg1 -176.16(16) . . . . ? C16 N2 C1 Mg1 0.5(3) . . . . ? C2 N1 C1 N2 0.0(3) . . . . ? C4 N1 C1 N2 -174.7(2) . . . . ? C2 N1 C1 Mg1 176.01(16) . . . . ? C4 N1 C1 Mg1 1.3(3) . . . . ? C40 Mg1 C1 N2 78.4(2) . . . . ? C30 Mg1 C1 N2 -49.2(2) . . . . ? C50 Mg1 C1 N2 -155.6(2) . . . . ? Mg2 Mg1 C1 N2 -101.73(19) . . . . ? C40 Mg1 C1 N1 -96.6(2) . . . . ? C30 Mg1 C1 N1 135.7(2) . . . . ? C50 Mg1 C1 N1 29.4(2) . . . . ? Mg2 Mg1 C1 N1 83.3(2) . . . . ? C1 N1 C2 C3 0.1(3) . . . . ? C4 N1 C2 C3 175.1(2) . . . . ? N1 C2 C3 N2 -0.2(3) . . . . ? C1 N2 C3 C2 0.3(3) . . . . ? C16 N2 C3 C2 -176.7(2) . . . . ? C1 N1 C4 C9 -103.2(3) . . . . ? C2 N1 C4 C9 82.6(3) . . . . ? C1 N1 C4 C5 80.2(3) . . . . ? C2 N1 C4 C5 -94.0(3) . . . . ? C9 C4 C5 C6 -2.1(4) . . . . ? N1 C4 C5 C6 174.3(2) . . . . ? C9 C4 C5 C10 -177.1(2) . . . . ? N1 C4 C5 C10 -0.8(3) . . . . ? C4 C5 C6 C7 1.4(4) . . . . ? C10 C5 C6 C7 176.6(2) . . . . ? C5 C6 C7 C8 -0.3(4) . . . . ? C6 C7 C8 C9 -0.1(4) . . . . ? C5 C4 C9 C8 1.6(4) . . . . ? N1 C4 C9 C8 -174.7(2) . . . . ? C5 C4 C9 C13 162.9(7) . . . . ? N1 C4 C9 C13 -13.5(8) . . . . ? C5 C4 C9 C13A -176.6(4) . . . . ? N1 C4 C9 C13A 7.1(4) . . . . ? C7 C8 C9 C4 -0.5(4) . . . . ? C7 C8 C9 C13 -161.7(8) . . . . ? C7 C8 C9 C13A 177.7(4) . . . . ? C4 C5 C10 C11 -139.0(2) . . . . ? C6 C5 C10 C11 46.0(3) . . . . ? C4 C5 C10 C12 96.3(3) . . . . ? C6 C5 C10 C12 -78.6(3) . . . . ? C1 N2 C16 C21 104.6(3) . . . . ? C3 N2 C16 C21 -79.0(3) . . . . ? C1 N2 C16 C17 -80.5(3) . . . . ? C3 N2 C16 C17 95.9(3) . . . . ? C21 C16 C17 C18 1.0(4) . . . . ? N2 C16 C17 C18 -173.5(2) . . . . ? C21 C16 C17 C22 177.3(2) . . . . ? N2 C16 C17 C22 2.8(3) . . . . ? C16 C17 C18 C19 -0.2(4) . . . . ? C22 C17 C18 C19 -176.6(3) . . . . ? C17 C18 C19 C20 -0.3(4) . . . . ? C18 C19 C20 C21 0.1(4) . . . . ? C17 C16 C21 C20 -1.2(4) . . . . ? N2 C16 C21 C20 173.3(2) . . . . ? C17 C16 C21 C25 -178.9(2) . . . . ? N2 C16 C21 C25 -4.4(4) . . . . ? C19 C20 C21 C16 0.6(4) . . . . ? C19 C20 C21 C25 178.4(3) . . . . ? C18 C17 C22 C24 -36.7(3) . . . . ? C16 C17 C22 C24 147.1(2) . . . . ? C18 C17 C22 C23 87.2(3) . . . . ? C16 C17 C22 C23 -89.0(3) . . . . ? C16 C21 C25 C26 -134.6(3) . . . . ? C20 C21 C25 C26 47.8(3) . . . . ? C16 C21 C25 C27 102.7(3) . . . . ? C20 C21 C25 C27 -74.9(3) . . . . ? C50 Mg2 C30 C31 114.7(2) . . . . ? C60 Mg2 C30 C31 -124.5(2) . . . . ? C60 Mg2 C30 C31 -10.0(3) 3_775 . . . ? Mg1 Mg2 C30 C31 102.1(3) . . . . ? Mg2 Mg2 C30 C31 -63.9(3) 3_775 . . . ? C51 Mg2 C30 C31 93.1(3) . . . . ? C50 Mg2 C30 Mg1 12.59(12) . . . . ? C60 Mg2 C30 Mg1 133.38(10) . . . . ? C60 Mg2 C30 Mg1 -112.11(10) 3_775 . . . ? Mg2 Mg2 C30 Mg1 -165.97(6) 3_775 . . . ? C51 Mg2 C30 Mg1 -8.98(16) . . . . ? C40 Mg1 C30 C31 -12.7(3) . . . . ? C1 Mg1 C30 C31 116.0(2) . . . . ? C50 Mg1 C30 C31 -133.3(2) . . . . ? Mg2 Mg1 C30 C31 -121.8(2) . . . . ? C40 Mg1 C30 Mg2 109.09(11) . . . . ? C1 Mg1 C30 Mg2 -122.20(9) . . . . ? C50 Mg1 C30 Mg2 -11.49(11) . . . . ? Mg2 C30 C31 C32 129.0(3) . . . . ? Mg1 C30 C31 C32 -147.6(2) . . . . ? C30 C31 C32 C33 178.2(3) . . . . ? C1 Mg1 C40 C41 146.65(19) . . . . ? C30 Mg1 C40 C41 -91.9(2) . . . . ? C50 Mg1 C40 C41 22.9(3) . . . . ? Mg2 Mg1 C40 C41 -33.2(3) . . . . ? Mg1 C40 C41 C42 175.34(19) . . . . ? C40 C41 C42 C43 -175.8(2) . . . . ? C30 Mg2 C50 C51 -149.70(18) . . . . ? C60 Mg2 C50 C51 86.47(19) . . . . ? C60 Mg2 C50 C51 -33.3(2) 3_775 . . . ? Mg1 Mg2 C50 C51 -137.3(2) . . . . ? Mg2 Mg2 C50 C51 28.7(2) 3_775 . . . ? C30 Mg2 C50 Mg1 -12.40(12) . . . . ? C60 Mg2 C50 Mg1 -136.22(9) . . . . ? C60 Mg2 C50 Mg1 104.06(10) 3_775 . . . ? Mg2 Mg2 C50 Mg1 166.01(7) 3_775 . . . ? C51 Mg2 C50 Mg1 137.3(2) . . . . ? C40 Mg1 C50 C51 -26.1(3) . . . . ? C1 Mg1 C50 C51 -155.2(3) . . . . ? C30 Mg1 C50 C51 97.1(3) . . . . ? Mg2 Mg1 C50 C51 85.5(3) . . . . ? C40 Mg1 C50 Mg2 -111.54(11) . . . . ? C1 Mg1 C50 Mg2 119.30(8) . . . . ? C30 Mg1 C50 Mg2 11.62(11) . . . . ? Mg2 C50 C51 C52 -151.6(2) . . . . ? Mg1 C50 C51 C52 132.7(3) . . . . ? Mg1 C50 C51 Mg2 -75.8(3) . . . . ? C50 Mg2 C51 C52 69.0(4) . . . . ? C30 Mg2 C51 C52 110.8(4) . . . . ? C60 Mg2 C51 C52 -34.0(4) . . . . ? C60 Mg2 C51 C52 -140.3(4) 3_775 . . . ? Mg1 Mg2 C51 C52 103.4(4) . . . . ? Mg2 Mg2 C51 C52 -89.0(4) 3_775 . . . ? C30 Mg2 C51 C50 41.8(2) . . . . ? C60 Mg2 C51 C50 -103.0(2) . . . . ? C60 Mg2 C51 C50 150.7(2) 3_775 . . . ? Mg1 Mg2 C51 C50 34.44(18) . . . . ? Mg2 Mg2 C51 C50 -157.96(19) 3_775 . . . ? C50 C51 C52 C53 68.6(3) . . . . ? Mg2 C51 C52 C53 15.8(6) . . . . ? C50 Mg2 C60 C61 99.05(19) . . . . ? C30 Mg2 C60 C61 -21.4(2) . . . . ? C60 Mg2 C60 C61 -134.6(2) 3_775 . . . ? Mg1 Mg2 C60 C61 40.6(2) . . . . ? Mg2 Mg2 C60 C61 -134.6(2) 3_775 . . . ? C51 Mg2 C60 C61 131.68(18) . . . . ? C50 Mg2 C60 Mg2 -126.34(10) . . . 3_775 ? C30 Mg2 C60 Mg2 113.22(11) . . . 3_775 ? C60 Mg2 C60 Mg2 0.0 3_775 . . 3_775 ? Mg1 Mg2 C60 Mg2 175.16(9) . . . 3_775 ? C51 Mg2 C60 Mg2 -93.71(9) . . . 3_775 ? Mg2 C60 C61 C62 -162.6(2) . . . . ? Mg2 C60 C61 C62 117.4(3) 3_775 . . . ? C60 C61 C62 C63 -179.6(3) . . . . ? C4 C9 C13 C14 -153.1(10) . . . . ? C8 C9 C13 C14 7.4(16) . . . . ? C13A C9 C13 C14 106(4) . . . . ? C4 C9 C13 C15 86.6(13) . . . . ? C8 C9 C13 C15 -112.9(11) . . . . ? C13A C9 C13 C15 -14(2) . . . . ? C4 C9 C13A C14A -104.2(5) . . . . ? C8 C9 C13A C14A 77.6(6) . . . . ? C13 C9 C13A C14A -14(3) . . . . ? C4 C9 C13A C15A 134.2(4) . . . . ? C8 C9 C13A C15A -43.9(6) . . . . ? C13 C9 C13A C15A -136(4) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 64.99 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.401 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.053 #===END #----------------------------------------------- #---------------COMPOUND 5------------------------ #---------------------------------------------- data_sdr1004 _database_code_depnum_ccdc_archive 'CCDC 775966' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H90 Cl2 Mg2 N4' _chemical_formula_weight 1010.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5268(3) _cell_length_b 14.3634(5) _cell_length_c 35.1522(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.089(2) _cell_angle_gamma 90.00 _cell_volume 6276.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 13127 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 29.07 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 0.161 _exptl_absorpt_correction_T_min 0.85001 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 36444 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0868 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12334 _reflns_number_gt 7550 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Both carbene ligands and one butyl are disordered, leaving this as a low grade structure. Where possible the disorder has been modeled over two sites, though some of the remaining atoms also show signs of unmodeled disorder. The severity of the problems meant that attempted anisotropic refinement of many atoms and refinement of sofs was unsuccessful. Despite this, the model contained herein does show the atomic connectivity of this species - and so it is fit for the purpose of the ms. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1084P)^2^+0.8913P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12334 _refine_ls_number_parameters 587 _refine_ls_number_restraints 118 _refine_ls_R_factor_all 0.1192 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.2065 _refine_ls_wR_factor_gt 0.1921 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg -0.30663(8) -0.17814(9) 0.39707(3) 0.0458(3) Uani 1 1 d . . . Mg2 Mg -0.52036(7) -0.21722(7) 0.32852(3) 0.0353(3) Uani 1 1 d . B . Cl1 Cl -0.49612(6) -0.13803(6) 0.38983(2) 0.0435(2) Uani 1 1 d . B . Cl2 Cl -0.32889(6) -0.24575(7) 0.33363(2) 0.0498(2) Uani 1 1 d . B . N1 N -0.24062(18) -0.3754(2) 0.44020(7) 0.0418(7) Uani 1 1 d . . . N2 N -0.32793(17) -0.29210(17) 0.47581(7) 0.0335(6) Uani 1 1 d . . . N3 N -0.54406(16) -0.10089(17) 0.24800(7) 0.0306(5) Uani 1 1 d . . . N4 N -0.66876(17) -0.06200(17) 0.28089(7) 0.0337(6) Uani 1 1 d . . . C1 C -0.2915(2) -0.2921(2) 0.44093(8) 0.0346(7) Uani 1 1 d . A . C2 C -0.2456(3) -0.4252(3) 0.47352(10) 0.0489(9) Uani 1 1 d . A . H2 H -0.2158 -0.4851 0.4794 0.059 Uiso 1 1 calc R . . C3 C -0.2997(2) -0.3740(2) 0.49574(9) 0.0448(8) Uani 1 1 d . A . H3 H -0.3163 -0.3900 0.5206 0.054 Uiso 1 1 calc R . . C4 C -0.1684(5) -0.3887(5) 0.41186(19) 0.0367(17) Uiso 0.50 1 d P A 1 C5 C -0.0620(5) -0.3564(5) 0.41756(18) 0.0398(15) Uiso 0.50 1 d PD A 1 C6 C -0.0030(7) -0.3821(7) 0.3871(3) 0.072(2) Uiso 0.50 1 d P A 1 H6 H 0.0683 -0.3593 0.3876 0.087 Uiso 0.50 1 calc PR A 1 C7 C -0.0428(7) -0.4371(7) 0.3577(3) 0.077(2) Uiso 0.50 1 d P A 1 H7 H 0.0034 -0.4542 0.3393 0.093 Uiso 0.50 1 calc PR A 1 C8 C -0.1455(6) -0.4692(6) 0.3529(2) 0.061(2) Uiso 0.50 1 d P A 1 H8 H -0.1711 -0.5060 0.3312 0.073 Uiso 0.50 1 calc PR A 1 C9 C -0.2147(5) -0.4465(5) 0.38122(19) 0.0419(16) Uiso 0.50 1 d PD A 1 C10 C -0.0182(6) -0.2968(5) 0.45126(19) 0.0479(19) Uiso 0.50 1 d PD A 1 H10 H -0.0810 -0.2759 0.4641 0.058 Uiso 0.50 1 calc PR A 1 C11 C 0.0363(6) -0.2109(6) 0.4390(2) 0.056(2) Uiso 0.50 1 d PD A 1 H11A H 0.1017 -0.2285 0.4281 0.085 Uiso 0.50 1 calc PR A 1 H11B H 0.0553 -0.1705 0.4613 0.085 Uiso 0.50 1 calc PR A 1 H11C H -0.0125 -0.1777 0.4197 0.085 Uiso 0.50 1 calc PR A 1 C12 C 0.0558(8) -0.3501(8) 0.4807(3) 0.074(3) Uiso 0.50 1 d PD A 1 H12A H 0.0165 -0.4022 0.4904 0.110 Uiso 0.50 1 calc PR A 1 H12B H 0.0819 -0.3087 0.5020 0.110 Uiso 0.50 1 calc PR A 1 H12C H 0.1171 -0.3741 0.4688 0.110 Uiso 0.50 1 calc PR A 1 C13 C -0.3320(6) -0.4834(6) 0.3757(2) 0.058(3) Uiso 0.50 1 d PD A 1 H13 H -0.3734 -0.4309 0.3854 0.070 Uiso 0.50 1 calc PR A 1 C14 C -0.3820(8) -0.4924(7) 0.3344(2) 0.058(2) Uiso 0.50 1 d PD A 1 H14A H -0.3405 -0.5370 0.3210 0.086 Uiso 0.50 1 calc PR A 1 H14B H -0.3816 -0.4316 0.3217 0.086 Uiso 0.50 1 calc PR A 1 H14C H -0.4562 -0.5145 0.3336 0.086 Uiso 0.50 1 calc PR A 1 C15 C -0.3679(6) -0.5688(6) 0.3986(2) 0.058 Uiso 0.50 1 d PD A 1 H15A H -0.4463 -0.5677 0.3983 0.086 Uiso 0.50 1 calc PR A 1 H15B H -0.3334 -0.5658 0.4251 0.086 Uiso 0.50 1 calc PR A 1 H15C H -0.3467 -0.6266 0.3867 0.086 Uiso 0.50 1 calc PR A 1 C16 C -0.3768(3) -0.2146(2) 0.49353(9) 0.0408(7) Uani 1 1 d U A . C17 C -0.3078(3) -0.1454(3) 0.51179(10) 0.0564(10) Uani 1 1 d DU . . C18 C -0.3568(4) -0.0752(3) 0.53082(11) 0.0764(13) Uani 1 1 d U A . H18 H -0.3138 -0.0265 0.5429 0.092 Uiso 1 1 calc R . . C19 C -0.4654(5) -0.0747(3) 0.53254(13) 0.0835(14) Uani 1 1 d U . . H19 H -0.4961 -0.0270 0.5464 0.100 Uiso 1 1 calc R A . C20 C -0.5297(3) -0.1419(3) 0.51461(11) 0.0671(11) Uani 1 1 d U A . H20 H -0.6048 -0.1403 0.5162 0.081 Uiso 1 1 calc R . . C21 C -0.4874(3) -0.2130(3) 0.49387(10) 0.0460(8) Uani 1 1 d U . . C22 C -0.1923(5) -0.1373(6) 0.5129(3) 0.052(3) Uiso 0.50 1 d PD A 1 H22 H -0.1705 -0.1680 0.4896 0.062 Uiso 0.50 1 calc PR A 1 C23 C -0.1425(7) -0.1917(7) 0.5482(2) 0.050(2) Uiso 0.50 1 d PD A 1 H23A H -0.1457 -0.1540 0.5713 0.076 Uiso 0.50 1 calc PR A 1 H23B H -0.0673 -0.2063 0.5456 0.076 Uiso 0.50 1 calc PR A 1 H23C H -0.1826 -0.2497 0.5503 0.076 Uiso 0.50 1 calc PR A 1 C24 C -0.1518(6) -0.0381(5) 0.5141(2) 0.0489(18) Uiso 0.50 1 d PD A 1 H24A H -0.1869 -0.0040 0.4919 0.073 Uiso 0.50 1 calc PR A 1 H24B H -0.0738 -0.0380 0.5136 0.073 Uiso 0.50 1 calc PR A 1 H24C H -0.1685 -0.0080 0.5377 0.073 Uiso 0.50 1 calc PR A 1 C25 C -0.5597(3) -0.2853(3) 0.47332(11) 0.0548(9) Uani 1 1 d . A . H25 H -0.5221 -0.3127 0.4525 0.066 Uiso 1 1 calc R . . C26 C -0.6675(3) -0.2450(4) 0.45515(12) 0.0769(14) Uani 1 1 d . . . H26A H -0.7110 -0.2276 0.4754 0.115 Uiso 1 1 calc R A . H26B H -0.7060 -0.2919 0.4385 0.115 Uiso 1 1 calc R . . H26C H -0.6544 -0.1898 0.4400 0.115 Uiso 1 1 calc R . . C27 C -0.5820(4) -0.3630(4) 0.50071(16) 0.0929(16) Uani 1 1 d . . . H27A H -0.5139 -0.3921 0.5113 0.139 Uiso 1 1 calc R A . H27B H -0.6286 -0.4099 0.4868 0.139 Uiso 1 1 calc R . . H27C H -0.6178 -0.3372 0.5216 0.139 Uiso 1 1 calc R . . C30 C -0.5761(2) -0.1133(2) 0.28296(8) 0.0302(6) Uani 1 1 d . B . C31 C -0.6143(2) -0.0442(2) 0.22477(9) 0.0431(8) Uani 1 1 d . B . H31 H -0.6079 -0.0260 0.1992 0.052 Uiso 1 1 calc R . . C32 C -0.6922(2) -0.0203(2) 0.24536(9) 0.0445(8) Uani 1 1 d . B . H32 H -0.7525 0.0180 0.2372 0.053 Uiso 1 1 calc R . . C33 C -0.4446(2) -0.1407(3) 0.23533(10) 0.0229(13) Uiso 0.65 1 d PG B 1 C34 C -0.45015(18) -0.2135(2) 0.20907(10) 0.0296(12) Uiso 0.65 1 d PG B 1 C35 C -0.3574(2) -0.2441(2) 0.19493(10) 0.0367(11) Uiso 0.65 1 d PG B 1 H35 H -0.3612 -0.2938 0.1770 0.044 Uiso 0.65 1 calc PR B 1 C36 C -0.25919(19) -0.2021(2) 0.20704(10) 0.0339(11) Uiso 0.65 1 d PG B 1 H36 H -0.1958 -0.2230 0.1974 0.041 Uiso 0.65 1 calc PR B 1 C37 C -0.2536(2) -0.1293(2) 0.23330(10) 0.0365(13) Uiso 0.65 1 d PG B 1 H37 H -0.1865 -0.1006 0.2416 0.044 Uiso 0.65 1 calc PR B 1 C38 C -0.3463(3) -0.0987(2) 0.24744(10) 0.0410(14) Uiso 0.65 1 d PGD B 1 C39 C -0.5553(4) -0.2633(4) 0.1954(2) 0.0380(16) Uiso 0.65 1 d P B 1 H39 H -0.6136 -0.2331 0.2081 0.046 Uiso 0.65 1 calc PR B 1 C40 C -0.5490(7) -0.3651(5) 0.2076(2) 0.053(2) Uiso 0.65 1 d P B 1 H40A H -0.6181 -0.3955 0.1996 0.080 Uiso 0.65 1 calc PR B 1 H40B H -0.5325 -0.3689 0.2356 0.080 Uiso 0.65 1 calc PR B 1 H40C H -0.4922 -0.3963 0.1956 0.080 Uiso 0.65 1 calc PR B 1 C41 C -0.5830(6) -0.2525(6) 0.1529(2) 0.0535(19) Uiso 0.65 1 d P B 1 H41A H -0.5851 -0.1862 0.1463 0.080 Uiso 0.65 1 calc PR B 1 H41B H -0.6536 -0.2805 0.1449 0.080 Uiso 0.65 1 calc PR B 1 H41C H -0.5285 -0.2838 0.1398 0.080 Uiso 0.65 1 calc PR B 1 C42 C -0.3394(4) -0.0219(4) 0.27866(15) 0.0509(13) Uiso 0.65 1 d PD B 1 H42 H -0.3906 -0.0381 0.2973 0.061 Uiso 0.65 1 calc PR B 1 C43 C -0.2300(4) -0.0060(4) 0.30068(16) 0.0552(15) Uiso 0.65 1 d PD B 1 H43A H -0.2061 -0.0628 0.3146 0.083 Uiso 0.65 1 calc PR B 1 H43B H -0.2341 0.0451 0.3189 0.083 Uiso 0.65 1 calc PR B 1 H43C H -0.1788 0.0101 0.2828 0.083 Uiso 0.65 1 calc PR B 1 C44 C -0.3754(5) 0.0690(5) 0.25931(19) 0.0689(18) Uiso 0.65 1 d PD B 1 H44A H -0.3256 0.0864 0.2411 0.103 Uiso 0.65 1 calc PR B 1 H44B H -0.3761 0.1179 0.2787 0.103 Uiso 0.65 1 calc PR B 1 H44C H -0.4479 0.0616 0.2456 0.103 Uiso 0.65 1 calc PR B 1 C45 C -0.7275(2) -0.0462(2) 0.31321(8) 0.0339(7) Uani 1 1 d . B . C46 C -0.6899(2) 0.0248(2) 0.33882(9) 0.0382(7) Uani 1 1 d . . . C47 C -0.7466(2) 0.0390(2) 0.36986(9) 0.0444(8) Uani 1 1 d . B . H47 H -0.7227 0.0852 0.3883 0.053 Uiso 1 1 calc R . . C48 C -0.8361(3) -0.0121(3) 0.37450(9) 0.0478(8) Uani 1 1 d . . . H48 H -0.8740 -0.0003 0.3958 0.057 Uiso 1 1 calc R B . C49 C -0.8723(2) -0.0812(2) 0.34836(9) 0.0444(8) Uani 1 1 d . B . H49 H -0.9346 -0.1162 0.3520 0.053 Uiso 1 1 calc R . . C50 C -0.8184(2) -0.0995(2) 0.31708(9) 0.0377(7) Uani 1 1 d . . . C51 C -0.5959(2) 0.0878(2) 0.33202(10) 0.0498(9) Uani 1 1 d . B . H51 H -0.5475 0.0510 0.3171 0.060 Uiso 1 1 calc R . . C52 C -0.6348(3) 0.1721(3) 0.30770(13) 0.0713(12) Uani 1 1 d . . . H52A H -0.6772 0.1511 0.2840 0.107 Uiso 1 1 calc R B . H52B H -0.5726 0.2078 0.3014 0.107 Uiso 1 1 calc R . . H52C H -0.6795 0.2116 0.3221 0.107 Uiso 1 1 calc R . . C53 C -0.5292(3) 0.1203(3) 0.36829(13) 0.0700(12) Uani 1 1 d . . . H53A H -0.5712 0.1643 0.3817 0.105 Uiso 1 1 calc R B . H53B H -0.4640 0.1511 0.3618 0.105 Uiso 1 1 calc R . . H53C H -0.5092 0.0667 0.3849 0.105 Uiso 1 1 calc R . . C54 C -0.8622(2) -0.1712(2) 0.28729(10) 0.0464(8) Uani 1 1 d . B . H54 H -0.8014 -0.1924 0.2735 0.056 Uiso 1 1 calc R . . C55 C -0.9468(3) -0.1246(3) 0.25796(12) 0.0692(12) Uani 1 1 d . . . H55A H -1.0046 -0.0989 0.2712 0.104 Uiso 1 1 calc R B . H55B H -0.9768 -0.1708 0.2391 0.104 Uiso 1 1 calc R . . H55C H -0.9130 -0.0743 0.2449 0.104 Uiso 1 1 calc R . . C56 C -0.9089(3) -0.2562(3) 0.30487(13) 0.0721(12) Uani 1 1 d . . . H56A H -0.8573 -0.2799 0.3258 0.108 Uiso 1 1 calc R B . H56B H -0.9238 -0.3046 0.2853 0.108 Uiso 1 1 calc R . . H56C H -0.9759 -0.2390 0.3148 0.108 Uiso 1 1 calc R . . C60 C -0.1879(4) -0.0772(3) 0.40325(15) 0.0396(10) Uiso 0.67 1 d PD C 1 H60A H -0.1373 -0.0914 0.4264 0.048 Uiso 0.67 1 calc PR C 1 H60B H -0.1471 -0.0802 0.3809 0.048 Uiso 0.67 1 calc PR C 1 C61 C -0.2303(4) 0.0212(3) 0.40660(15) 0.0459(11) Uiso 0.67 1 d PD C 1 H61A H -0.2685 0.0239 0.4296 0.055 Uiso 0.67 1 calc PR C 1 H61B H -0.2841 0.0331 0.3841 0.055 Uiso 0.67 1 calc PR C 1 C62 C -0.1469(4) 0.1010(3) 0.40938(17) 0.0521(12) Uiso 0.67 1 d PD C 1 H62A H -0.0927 0.0893 0.4318 0.063 Uiso 0.67 1 calc PR C 1 H62B H -0.1092 0.0992 0.3862 0.063 Uiso 0.67 1 calc PR C 1 C63 C -0.1930(6) 0.1990(5) 0.4131(2) 0.0838(19) Uiso 0.67 1 d PD C 1 H63A H -0.2458 0.2122 0.3908 0.126 Uiso 0.67 1 calc PR C 1 H63B H -0.1346 0.2448 0.4143 0.126 Uiso 0.67 1 calc PR C 1 H63C H -0.2279 0.2028 0.4365 0.126 Uiso 0.67 1 calc PR C 1 C70 C -0.6180(2) -0.3392(2) 0.32319(8) 0.0345(7) Uani 1 1 d . . . H70A H -0.6895 -0.3229 0.3096 0.041 Uiso 1 1 calc R C . H70B H -0.5848 -0.3853 0.3073 0.041 Uiso 1 1 calc R . . C71 C -0.6336(3) -0.3849(2) 0.36223(9) 0.0457(8) Uani 1 1 d . C . H71A H -0.5616 -0.3971 0.3763 0.055 Uiso 1 1 calc R . . H71B H -0.6698 -0.3392 0.3774 0.055 Uiso 1 1 calc R . . C72 C -0.6981(3) -0.4757(3) 0.36055(10) 0.0572(10) Uani 1 1 d . . . H72A H -0.7724 -0.4629 0.3486 0.069 Uiso 1 1 calc R C . H72B H -0.6655 -0.5204 0.3439 0.069 Uiso 1 1 calc R . . C73 C -0.7029(4) -0.5201(4) 0.39926(12) 0.0844(14) Uani 1 1 d . C . H73A H -0.6305 -0.5394 0.4102 0.127 Uiso 1 1 calc R . . H73B H -0.7501 -0.5747 0.3963 0.127 Uiso 1 1 calc R . . H73C H -0.7312 -0.4751 0.4164 0.127 Uiso 1 1 calc R . . C4A C -0.1830(3) -0.4212(4) 0.41081(14) 0.042(2) Uiso 0.50 1 d PG A 2 C5A C -0.0743(4) -0.3993(3) 0.41359(13) 0.0433(17) Uiso 0.50 1 d PGD A 2 C6A C -0.0091(3) -0.4428(4) 0.38969(16) 0.065(2) Uiso 0.50 1 d PG A 2 H6A H 0.0653 -0.4279 0.3916 0.078 Uiso 0.50 1 calc PR A 2 C7A C -0.0527(4) -0.5082(4) 0.36302(15) 0.086(3) Uiso 0.50 1 d PG A 2 H7A H -0.0081 -0.5379 0.3467 0.103 Uiso 0.50 1 calc PR A 2 C8A C -0.1614(4) -0.5300(4) 0.36023(16) 0.082(3) Uiso 0.50 1 d PG A 2 H8A H -0.1912 -0.5747 0.3420 0.098 Uiso 0.50 1 calc PR A 2 C9A C -0.2266(3) -0.4865(4) 0.38413(16) 0.069(3) Uiso 0.50 1 d PGD A 2 C10A C -0.0216(5) -0.3337(5) 0.4433(2) 0.0487(19) Uiso 0.50 1 d PD A 2 H10A H -0.0787 -0.3067 0.4575 0.058 Uiso 0.50 1 calc PR A 2 C11A C 0.0359(7) -0.2533(6) 0.4257(3) 0.075(3) Uiso 0.50 1 d PD A 2 H11D H 0.0957 -0.2779 0.4131 0.112 Uiso 0.50 1 calc PR A 2 H11E H 0.0638 -0.2095 0.4459 0.112 Uiso 0.50 1 calc PR A 2 H11F H -0.0149 -0.2210 0.4067 0.112 Uiso 0.50 1 calc PR A 2 C12A C 0.0604(7) -0.3835(7) 0.4723(3) 0.065(3) Uiso 0.50 1 d PD A 2 H12D H 0.0244 -0.4333 0.4849 0.098 Uiso 0.50 1 calc PR A 2 H12E H 0.0918 -0.3388 0.4916 0.098 Uiso 0.50 1 calc PR A 2 H12F H 0.1175 -0.4102 0.4590 0.098 Uiso 0.50 1 calc PR A 2 C13A C -0.3429(7) -0.5085(8) 0.3822(3) 0.087(4) Uiso 0.50 1 d PD A 2 H13A H -0.3823 -0.4696 0.3995 0.105 Uiso 0.50 1 calc PR A 2 C15A C -0.3160(8) -0.6046(7) 0.3971(3) 0.087 Uiso 0.50 1 d PD A 2 H15D H -0.2756 -0.6377 0.3791 0.131 Uiso 0.50 1 calc PR A 2 H15E H -0.3826 -0.6385 0.3997 0.131 Uiso 0.50 1 calc PR A 2 H15F H -0.2722 -0.6004 0.4221 0.131 Uiso 0.50 1 calc PR A 2 C14A C -0.3985(10) -0.5171(9) 0.3422(3) 0.084(4) Uiso 0.50 1 d PD A 2 H14D H -0.3686 -0.5700 0.3295 0.127 Uiso 0.50 1 calc PR A 2 H14E H -0.3878 -0.4599 0.3280 0.127 Uiso 0.50 1 calc PR A 2 H14F H -0.4757 -0.5271 0.3430 0.127 Uiso 0.50 1 calc PR A 2 C22A C -0.1842(5) -0.1612(7) 0.5109(3) 0.059(3) Uiso 0.50 1 d PD A 2 H22A H -0.1768 -0.1965 0.4869 0.071 Uiso 0.50 1 calc PR A 2 C23A C -0.1295(8) -0.2201(7) 0.5441(3) 0.065(3) Uiso 0.50 1 d PD A 2 H23D H -0.0516 -0.2208 0.5432 0.097 Uiso 0.50 1 calc PR A 2 H23E H -0.1572 -0.2839 0.5418 0.097 Uiso 0.50 1 calc PR A 2 H23F H -0.1446 -0.1934 0.5685 0.097 Uiso 0.50 1 calc PR A 2 C24A C -0.1154(7) -0.0726(6) 0.5096(3) 0.066(2) Uiso 0.50 1 d PD A 2 H24D H -0.1084 -0.0418 0.5347 0.099 Uiso 0.50 1 calc PR A 2 H24E H -0.1502 -0.0302 0.4900 0.099 Uiso 0.50 1 calc PR A 2 H24F H -0.0439 -0.0895 0.5033 0.099 Uiso 0.50 1 calc PR A 2 C42A C -0.3564(6) 0.0215(5) 0.2644(2) 0.0278(17) Uiso 0.35 1 d PD B 2 H42A H -0.4336 0.0352 0.2666 0.033 Uiso 0.35 1 calc PR B 2 C43A C -0.3224(6) 0.0955(6) 0.2372(2) 0.0313(18) Uiso 0.35 1 d PD B 2 H43D H -0.3284 0.1573 0.2486 0.047 Uiso 0.35 1 calc PR B 2 H43E H -0.3694 0.0923 0.2128 0.047 Uiso 0.35 1 calc PR B 2 H43F H -0.2478 0.0845 0.2327 0.047 Uiso 0.35 1 calc PR B 2 C44A C -0.2995(8) 0.0306(8) 0.3048(2) 0.052(2) Uiso 0.35 1 d PD B 2 H44D H -0.2221 0.0206 0.3046 0.078 Uiso 0.35 1 calc PR B 2 H44E H -0.3278 -0.0160 0.3213 0.078 Uiso 0.35 1 calc PR B 2 H44F H -0.3117 0.0931 0.3146 0.078 Uiso 0.35 1 calc PR B 2 C60A C -0.2060(8) -0.0458(7) 0.4105(3) 0.0396(10) Uiso 0.33 1 d PD C 2 H60C H -0.1552 -0.0589 0.4338 0.048 Uiso 0.33 1 calc PR C 2 H60D H -0.1620 -0.0370 0.3892 0.048 Uiso 0.33 1 calc PR C 2 C61A C -0.2588(8) 0.0465(6) 0.4168(3) 0.0459(11) Uiso 0.33 1 d PD C 2 H61C H -0.3096 0.0366 0.4359 0.055 Uiso 0.33 1 calc PR C 2 H61D H -0.3022 0.0642 0.3924 0.055 Uiso 0.33 1 calc PR C 2 C62A C -0.1873(8) 0.1302(7) 0.4303(3) 0.0521(12) Uiso 0.33 1 d PD C 2 H62C H -0.2289 0.1780 0.4424 0.063 Uiso 0.33 1 calc PR C 2 H62D H -0.1255 0.1105 0.4488 0.063 Uiso 0.33 1 calc PR C 2 C63A C -0.1507(12) 0.1662(12) 0.3948(4) 0.0838(19) Uiso 0.33 1 d PD C 2 H63D H -0.1128 0.1168 0.3826 0.126 Uiso 0.33 1 calc PR C 2 H63E H -0.1018 0.2189 0.4010 0.126 Uiso 0.33 1 calc PR C 2 H63F H -0.2130 0.1868 0.3772 0.126 Uiso 0.33 1 calc PR C 2 C33A C -0.4496(3) -0.1262(4) 0.2393(2) 0.031(3) Uiso 0.35 1 d PG B 2 C34A C -0.4448(3) -0.2114(4) 0.22091(19) 0.0248(19) Uiso 0.35 1 d PGD B 2 C35A C -0.3463(4) -0.2465(3) 0.21322(19) 0.036(2) Uiso 0.35 1 d PG B 2 H35A H -0.3430 -0.3048 0.2006 0.043 Uiso 0.35 1 calc PR B 2 C36A C -0.2525(3) -0.1963(4) 0.22395(19) 0.0292(18) Uiso 0.35 1 d PG B 2 H36A H -0.1852 -0.2202 0.2187 0.035 Uiso 0.35 1 calc PR B 2 C37A C -0.2573(4) -0.1110(4) 0.24238(19) 0.032(2) Uiso 0.35 1 d PG B 2 H37A H -0.1932 -0.0767 0.2497 0.039 Uiso 0.35 1 calc PR B 2 C38A C -0.3558(5) -0.0760(4) 0.2501(2) 0.025(2) Uiso 0.35 1 d PGD B 2 C39A C -0.5473(7) -0.2691(6) 0.2078(3) 0.033(3) Uiso 0.35 1 d PD B 2 H39A H -0.6047 -0.2455 0.2227 0.040 Uiso 0.35 1 calc PR B 2 C40A C -0.5342(12) -0.3732(7) 0.2170(4) 0.051(4) Uiso 0.35 1 d PD B 2 H40D H -0.4865 -0.4015 0.2002 0.077 Uiso 0.35 1 calc PR B 2 H40E H -0.6047 -0.4036 0.2130 0.077 Uiso 0.35 1 calc PR B 2 H40F H -0.5031 -0.3809 0.2438 0.077 Uiso 0.35 1 calc PR B 2 C41A C -0.5873(12) -0.2507(12) 0.1649(4) 0.063(4) Uiso 0.35 1 d PD B 2 H41D H -0.5331 -0.2724 0.1491 0.094 Uiso 0.35 1 calc PR B 2 H41E H -0.5992 -0.1838 0.1609 0.094 Uiso 0.35 1 calc PR B 2 H41F H -0.6549 -0.2842 0.1577 0.094 Uiso 0.35 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0326(5) 0.0616(8) 0.0405(6) 0.0247(6) -0.0065(4) -0.0103(5) Mg2 0.0312(5) 0.0366(6) 0.0365(6) 0.0075(5) -0.0024(4) -0.0042(4) Cl1 0.0405(4) 0.0462(5) 0.0405(4) 0.0030(4) -0.0078(3) 0.0040(4) Cl2 0.0340(4) 0.0716(6) 0.0442(5) 0.0200(4) 0.0064(3) 0.0033(4) N1 0.0283(13) 0.0599(19) 0.0388(15) 0.0134(13) 0.0104(10) 0.0125(12) N2 0.0281(12) 0.0389(15) 0.0337(13) 0.0106(12) 0.0049(10) -0.0031(11) N3 0.0206(11) 0.0350(14) 0.0352(13) 0.0046(11) -0.0008(9) -0.0007(10) N4 0.0267(12) 0.0388(15) 0.0343(13) 0.0033(12) -0.0017(10) 0.0013(11) C1 0.0162(13) 0.0506(19) 0.0370(16) 0.0137(15) 0.0035(11) 0.0004(13) C2 0.0456(18) 0.048(2) 0.054(2) 0.0212(18) 0.0109(16) 0.0129(16) C3 0.0464(18) 0.049(2) 0.0402(18) 0.0216(16) 0.0100(14) -0.0027(16) C16 0.0477(18) 0.0398(18) 0.0341(17) 0.0060(14) 0.0020(13) -0.0003(15) C17 0.079(2) 0.053(2) 0.0326(18) 0.0090(17) -0.0108(16) -0.0167(19) C18 0.120(3) 0.049(2) 0.051(2) -0.010(2) -0.026(2) -0.006(2) C19 0.119(4) 0.067(3) 0.057(3) -0.018(2) -0.019(3) 0.023(3) C20 0.072(2) 0.069(3) 0.057(2) -0.010(2) -0.0007(19) 0.025(2) C21 0.0440(18) 0.050(2) 0.0441(19) -0.0018(16) 0.0046(14) 0.0067(16) C25 0.0358(18) 0.070(3) 0.061(2) -0.009(2) 0.0155(15) -0.0032(17) C26 0.0327(19) 0.127(4) 0.073(3) -0.024(3) 0.0124(17) 0.003(2) C27 0.072(3) 0.092(4) 0.116(4) 0.009(3) 0.018(3) -0.024(3) C30 0.0211(13) 0.0316(16) 0.0365(16) 0.0003(13) -0.0014(11) -0.0056(12) C31 0.0331(16) 0.058(2) 0.0363(17) 0.0142(16) -0.0040(13) 0.0082(15) C32 0.0322(16) 0.059(2) 0.0396(18) 0.0098(16) -0.0066(13) 0.0124(15) C45 0.0261(14) 0.0385(17) 0.0358(16) 0.0031(14) -0.0012(12) 0.0040(13) C46 0.0330(16) 0.0378(18) 0.0421(18) 0.0025(15) -0.0026(13) 0.0072(14) C47 0.0438(18) 0.047(2) 0.0404(18) -0.0044(16) -0.0028(14) 0.0040(16) C48 0.0468(19) 0.057(2) 0.0402(19) -0.0022(17) 0.0087(14) 0.0066(17) C49 0.0379(17) 0.051(2) 0.0451(19) 0.0027(17) 0.0077(14) -0.0008(15) C50 0.0311(15) 0.0362(18) 0.0452(18) 0.0018(15) 0.0021(13) 0.0004(13) C51 0.0362(17) 0.049(2) 0.063(2) -0.0106(18) 0.0043(15) -0.0045(16) C52 0.072(3) 0.064(3) 0.077(3) 0.019(2) 0.005(2) -0.019(2) C53 0.061(2) 0.055(2) 0.087(3) -0.001(2) -0.016(2) -0.017(2) C54 0.0290(16) 0.052(2) 0.059(2) -0.0142(18) 0.0062(14) -0.0037(15) C55 0.040(2) 0.087(3) 0.075(3) -0.033(2) -0.0144(18) 0.011(2) C56 0.057(2) 0.064(3) 0.101(3) -0.025(2) 0.030(2) -0.025(2) C70 0.0311(15) 0.0313(17) 0.0406(17) 0.0000(14) 0.0020(12) -0.0068(13) C71 0.0421(17) 0.050(2) 0.0438(19) 0.0000(16) -0.0003(14) -0.0113(16) C72 0.060(2) 0.059(2) 0.051(2) 0.0067(19) 0.0010(17) -0.0244(19) C73 0.093(3) 0.093(4) 0.065(3) 0.025(3) 0.002(2) -0.038(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 C60 2.069(5) . ? Mg1 C1 2.241(3) . ? Mg1 C60A 2.298(10) . ? Mg1 Cl2 2.4166(15) . ? Mg1 Cl1 2.4252(12) . ? Mg1 Mg2 3.4200(13) . ? Mg2 C70 2.132(3) . ? Mg2 C30 2.237(3) . ? Mg2 Cl2 2.4179(11) . ? Mg2 Cl1 2.4226(13) . ? N1 C1 1.357(4) . ? N1 C2 1.381(4) . ? N1 C4 1.439(7) . ? N1 C4A 1.485(5) . ? N2 C1 1.360(4) . ? N2 C3 1.392(4) . ? N2 C16 1.448(4) . ? N3 C33A 1.310(5) . ? N3 C30 1.351(4) . ? N3 C31 1.388(4) . ? N3 C33 1.489(3) . ? N4 C30 1.370(3) . ? N4 C32 1.383(4) . ? N4 C45 1.446(4) . ? C2 C3 1.320(5) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.403(9) . ? C4 C9 1.425(9) . ? C5 C6 1.422(10) . ? C5 C10 1.509(7) . ? C6 C7 1.348(12) . ? C6 H6 0.9500 . ? C7 C8 1.358(11) . ? C7 H7 0.9500 . ? C8 C9 1.435(10) . ? C8 H8 0.9500 . ? C9 C13 1.552(7) . ? C10 C11 1.498(7) . ? C10 C12 1.510(8) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.514(8) . ? C13 C15 1.564(8) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.387(5) . ? C16 C17 1.417(5) . ? C17 C18 1.394(6) . ? C17 C22 1.448(7) . ? C17 C22A 1.569(6) . ? C18 C19 1.369(7) . ? C18 H18 0.9500 . ? C19 C20 1.361(6) . ? C19 H19 0.9500 . ? C20 C21 1.397(5) . ? C20 H20 0.9500 . ? C21 C25 1.503(5) . ? C22 C24 1.510(8) . ? C22 C23 1.533(8) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.523(6) . ? C25 C26 1.534(5) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C31 C32 1.330(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C34 C39 1.524(6) . ? C35 C36 1.3900 . ? C35 H35 0.9500 . ? C36 C37 1.3900 . ? C36 H36 0.9500 . ? C37 C38 1.3900 . ? C37 H37 0.9500 . ? C38 C42 1.550(5) . ? C39 C41 1.500(10) . ? C39 C40 1.522(9) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.506(6) . ? C42 C44 1.516(7) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.393(4) . ? C45 C46 1.402(4) . ? C46 C47 1.389(4) . ? C46 C51 1.526(4) . ? C47 C48 1.366(5) . ? C47 H47 0.9500 . ? C48 C49 1.390(5) . ? C48 H48 0.9500 . ? C49 C50 1.384(4) . ? C49 H49 0.9500 . ? C50 C54 1.522(4) . ? C51 C53 1.510(5) . ? C51 C52 1.527(5) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C56 1.517(5) . ? C54 C55 1.538(5) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C60 C61 1.519(6) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.545(6) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.534(7) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C70 C71 1.555(4) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.532(5) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.511(5) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C4A C5A 1.3900 . ? C4A C9A 1.3900 . ? C5A C6A 1.3900 . ? C5A C10A 1.498(7) . ? C6A C7A 1.3900 . ? C6A H6A 0.9500 . ? C7A C8A 1.3900 . ? C7A H7A 0.9500 . ? C8A C9A 1.3900 . ? C8A H8A 0.9500 . ? C9A C13A 1.483(8) . ? C10A C12A 1.532(7) . ? C10A C11A 1.532(8) . ? C10A H10A 1.0000 . ? C11A H11D 0.9800 . ? C11A H11E 0.9800 . ? C11A H11F 0.9800 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A C14A 1.496(8) . ? C13A C15A 1.499(9) . ? C13A H13A 1.0000 . ? C15A H15D 0.9800 . ? C15A H15E 0.9800 . ? C15A H15F 0.9800 . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C22A C23A 1.532(8) . ? C22A C24A 1.540(8) . ? C22A H22A 1.0000 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C42A C38A 1.487(7) . ? C42A C44A 1.514(8) . ? C42A C43A 1.525(8) . ? C42A H42A 1.0000 . ? C43A H43D 0.9800 . ? C43A H43E 0.9800 . ? C43A H43F 0.9800 . ? C44A H44D 0.9800 . ? C44A H44E 0.9800 . ? C44A H44F 0.9800 . ? C60A C61A 1.510(9) . ? C60A H60C 0.9900 . ? C60A H60D 0.9900 . ? C61A C62A 1.539(8) . ? C61A H61C 0.9900 . ? C61A H61D 0.9900 . ? C62A C63A 1.474(9) . ? C62A H62C 0.9900 . ? C62A H62D 0.9900 . ? C63A H63D 0.9800 . ? C63A H63E 0.9800 . ? C63A H63F 0.9800 . ? C33A C34A 1.3900 . ? C33A C38A 1.3900 . ? C34A C35A 1.3900 . ? C34A C39A 1.551(7) . ? C35A C36A 1.3900 . ? C35A H35A 0.9500 . ? C36A C37A 1.3900 . ? C36A H36A 0.9500 . ? C37A C38A 1.3900 . ? C37A H37A 0.9500 . ? C39A C40A 1.534(9) . ? C39A C41A 1.550(9) . ? C39A H39A 1.0000 . ? C40A H40D 0.9800 . ? C40A H40E 0.9800 . ? C40A H40F 0.9800 . ? C41A H41D 0.9800 . ? C41A H41E 0.9800 . ? C41A H41F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C60 Mg1 C1 116.16(16) . . ? C60 Mg1 C60A 14.0(3) . . ? C1 Mg1 C60A 117.7(3) . . ? C60 Mg1 Cl2 112.21(15) . . ? C1 Mg1 Cl2 109.37(10) . . ? C60A Mg1 Cl2 121.3(3) . . ? C60 Mg1 Cl1 121.74(14) . . ? C1 Mg1 Cl1 104.16(8) . . ? C60A Mg1 Cl1 109.3(2) . . ? Cl2 Mg1 Cl1 89.92(4) . . ? C60 Mg1 Mg2 132.77(15) . . ? C1 Mg1 Mg2 110.94(8) . . ? C60A Mg1 Mg2 130.0(3) . . ? Cl2 Mg1 Mg2 44.99(3) . . ? Cl1 Mg1 Mg2 45.10(3) . . ? C70 Mg2 C30 111.12(11) . . ? C70 Mg2 Cl2 114.87(9) . . ? C30 Mg2 Cl2 112.66(8) . . ? C70 Mg2 Cl1 118.14(9) . . ? C30 Mg2 Cl1 108.51(9) . . ? Cl2 Mg2 Cl1 89.95(4) . . ? C70 Mg2 Mg1 125.99(9) . . ? C30 Mg2 Mg1 122.88(8) . . ? Cl2 Mg2 Mg1 44.96(3) . . ? Cl1 Mg2 Mg1 45.16(3) . . ? Mg2 Cl1 Mg1 89.74(4) . . ? Mg1 Cl2 Mg2 90.05(4) . . ? C1 N1 C2 111.7(3) . . ? C1 N1 C4 117.9(4) . . ? C2 N1 C4 128.1(4) . . ? C1 N1 C4A 132.3(3) . . ? C2 N1 C4A 115.9(3) . . ? C1 N2 C3 111.1(3) . . ? C1 N2 C16 126.5(2) . . ? C3 N2 C16 121.9(2) . . ? C33A N3 C30 123.6(4) . . ? C33A N3 C31 123.4(4) . . ? C30 N3 C31 112.0(2) . . ? C30 N3 C33 125.1(2) . . ? C31 N3 C33 122.9(3) . . ? C30 N4 C32 111.4(2) . . ? C30 N4 C45 123.6(2) . . ? C32 N4 C45 124.7(2) . . ? N1 C1 N2 103.2(2) . . ? N1 C1 Mg1 129.1(2) . . ? N2 C1 Mg1 127.6(2) . . ? C3 C2 N1 107.1(3) . . ? C3 C2 H2 126.5 . . ? N1 C2 H2 126.5 . . ? C2 C3 N2 106.9(3) . . ? C2 C3 H3 126.6 . . ? N2 C3 H3 126.6 . . ? C5 C4 C9 126.3(6) . . ? C5 C4 N1 121.6(6) . . ? C9 C4 N1 111.7(5) . . ? C4 C5 C6 112.3(6) . . ? C4 C5 C10 123.2(6) . . ? C6 C5 C10 124.4(6) . . ? C7 C6 C5 123.6(8) . . ? C7 C6 H6 118.2 . . ? C5 C6 H6 118.2 . . ? C6 C7 C8 123.3(9) . . ? C6 C7 H7 118.4 . . ? C8 C7 H7 118.4 . . ? C7 C8 C9 118.8(7) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C4 C9 C8 115.6(6) . . ? C4 C9 C13 125.8(6) . . ? C8 C9 C13 118.6(6) . . ? C11 C10 C5 112.1(6) . . ? C11 C10 C12 110.6(7) . . ? C5 C10 C12 112.5(7) . . ? C11 C10 H10 107.1 . . ? C5 C10 H10 107.1 . . ? C12 C10 H10 107.1 . . ? C14 C13 C9 115.0(7) . . ? C14 C13 C15 108.4(7) . . ? C9 C13 C15 122.1(6) . . ? C14 C13 H13 102.8 . . ? C9 C13 H13 102.8 . . ? C15 C13 H13 102.8 . . ? C21 C16 C17 122.6(3) . . ? C21 C16 N2 119.5(3) . . ? C17 C16 N2 117.9(3) . . ? C18 C17 C16 116.4(3) . . ? C18 C17 C22 115.2(5) . . ? C16 C17 C22 128.4(5) . . ? C18 C17 C22A 127.4(5) . . ? C16 C17 C22A 116.0(5) . . ? C19 C18 C17 121.6(4) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C20 C19 C18 120.7(4) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 121.3(4) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C16 C21 C20 117.4(3) . . ? C16 C21 C25 121.8(3) . . ? C20 C21 C25 120.8(3) . . ? C17 C22 C24 114.1(6) . . ? C17 C22 C23 106.7(6) . . ? C24 C22 C23 110.9(7) . . ? C17 C22 H22 108.3 . . ? C24 C22 H22 108.3 . . ? C23 C22 H22 108.3 . . ? C21 C25 C27 110.5(3) . . ? C21 C25 C26 112.8(3) . . ? C27 C25 C26 108.6(3) . . ? C21 C25 H25 108.3 . . ? C27 C25 H25 108.3 . . ? C26 C25 H25 108.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C30 N4 103.0(2) . . ? N3 C30 Mg2 129.7(2) . . ? N4 C30 Mg2 125.8(2) . . ? C32 C31 N3 106.6(3) . . ? C32 C31 H31 126.7 . . ? N3 C31 H31 126.7 . . ? C31 C32 N4 107.0(3) . . ? C31 C32 H32 126.5 . . ? N4 C32 H32 126.5 . . ? C34 C33 C38 120.0 . . ? C34 C33 N3 120.8(2) . . ? C38 C33 N3 118.9(2) . . ? C35 C34 C33 120.0 . . ? C35 C34 C39 117.8(3) . . ? C33 C34 C39 122.2(3) . . ? C34 C35 C36 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C33 120.0 . . ? C37 C38 C42 120.2(3) . . ? C33 C38 C42 119.7(3) . . ? C41 C39 C40 112.2(6) . . ? C41 C39 C34 110.5(5) . . ? C40 C39 C34 110.5(5) . . ? C41 C39 H39 107.8 . . ? C40 C39 H39 107.8 . . ? C34 C39 H39 107.8 . . ? C43 C42 C44 107.5(5) . . ? C43 C42 C38 116.1(4) . . ? C44 C42 C38 107.9(5) . . ? C43 C42 H42 108.4 . . ? C44 C42 H42 108.4 . . ? C38 C42 H42 108.4 . . ? C50 C45 C46 123.4(3) . . ? C50 C45 N4 119.5(3) . . ? C46 C45 N4 117.1(3) . . ? C47 C46 C45 116.6(3) . . ? C47 C46 C51 121.0(3) . . ? C45 C46 C51 122.3(3) . . ? C48 C47 C46 121.5(3) . . ? C48 C47 H47 119.3 . . ? C46 C47 H47 119.3 . . ? C47 C48 C49 120.7(3) . . ? C47 C48 H48 119.7 . . ? C49 C48 H48 119.7 . . ? C50 C49 C48 120.6(3) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C49 C50 C45 117.3(3) . . ? C49 C50 C54 120.3(3) . . ? C45 C50 C54 122.3(3) . . ? C53 C51 C46 114.1(3) . . ? C53 C51 C52 109.4(3) . . ? C46 C51 C52 111.0(3) . . ? C53 C51 H51 107.3 . . ? C46 C51 H51 107.3 . . ? C52 C51 H51 107.3 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C56 C54 C50 112.9(3) . . ? C56 C54 C55 110.8(3) . . ? C50 C54 C55 109.0(3) . . ? C56 C54 H54 108.0 . . ? C50 C54 H54 108.0 . . ? C55 C54 H54 108.0 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C61 C60 Mg1 114.0(3) . . ? C61 C60 H60A 108.8 . . ? Mg1 C60 H60A 108.8 . . ? C61 C60 H60B 108.8 . . ? Mg1 C60 H60B 108.8 . . ? H60A C60 H60B 107.7 . . ? C60 C61 C62 117.1(4) . . ? C60 C61 H61A 108.0 . . ? C62 C61 H61A 108.0 . . ? C60 C61 H61B 108.0 . . ? C62 C61 H61B 108.0 . . ? H61A C61 H61B 107.3 . . ? C63 C62 C61 115.4(5) . . ? C63 C62 H62A 108.4 . . ? C61 C62 H62A 108.4 . . ? C63 C62 H62B 108.4 . . ? C61 C62 H62B 108.4 . . ? H62A C62 H62B 107.5 . . ? C71 C70 Mg2 113.72(19) . . ? C71 C70 H70A 108.8 . . ? Mg2 C70 H70A 108.8 . . ? C71 C70 H70B 108.8 . . ? Mg2 C70 H70B 108.8 . . ? H70A C70 H70B 107.7 . . ? C72 C71 C70 116.7(3) . . ? C72 C71 H71A 108.1 . . ? C70 C71 H71A 108.1 . . ? C72 C71 H71B 108.1 . . ? C70 C71 H71B 108.1 . . ? H71A C71 H71B 107.3 . . ? C73 C72 C71 113.9(3) . . ? C73 C72 H72A 108.8 . . ? C71 C72 H72A 108.8 . . ? C73 C72 H72B 108.8 . . ? C71 C72 H72B 108.8 . . ? H72A C72 H72B 107.7 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C5A C4A C9A 120.0 . . ? C5A C4A N1 114.0(3) . . ? C9A C4A N1 125.8(3) . . ? C6A C5A C4A 120.0 . . ? C6A C5A C10A 117.6(4) . . ? C4A C5A C10A 122.3(4) . . ? C5A C6A C7A 120.0 . . ? C5A C6A H6A 120.0 . . ? C7A C6A H6A 120.0 . . ? C8A C7A C6A 120.0 . . ? C8A C7A H7A 120.0 . . ? C6A C7A H7A 120.0 . . ? C7A C8A C9A 120.0 . . ? C7A C8A H8A 120.0 . . ? C9A C8A H8A 120.0 . . ? C8A C9A C4A 120.0 . . ? C8A C9A C13A 121.6(6) . . ? C4A C9A C13A 118.4(6) . . ? C5A C10A C12A 111.8(6) . . ? C5A C10A C11A 112.4(6) . . ? C12A C10A C11A 108.1(7) . . ? C5A C10A H10A 108.1 . . ? C12A C10A H10A 108.1 . . ? C11A C10A H10A 108.1 . . ? C10A C11A H11D 109.5 . . ? C10A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? C10A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? C10A C12A H12D 109.5 . . ? C10A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C10A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C9A C13A C14A 113.6(9) . . ? C9A C13A C15A 90.2(7) . . ? C14A C13A C15A 108.1(10) . . ? C9A C13A H13A 114.2 . . ? C14A C13A H13A 114.2 . . ? C15A C13A H13A 114.2 . . ? C13A C15A H15D 109.5 . . ? C13A C15A H15E 109.5 . . ? H15D C15A H15E 109.5 . . ? C13A C15A H15F 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? C13A C14A H14D 109.5 . . ? C13A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C13A C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C23A C22A C24A 106.3(7) . . ? C23A C22A C17 114.5(7) . . ? C24A C22A C17 116.0(7) . . ? C23A C22A H22A 106.5 . . ? C24A C22A H22A 106.5 . . ? C17 C22A H22A 106.5 . . ? C22A C23A H23D 109.5 . . ? C22A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C22A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C22A C24A H24D 109.5 . . ? C22A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C22A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C38A C42A C44A 112.2(7) . . ? C38A C42A C43A 115.5(6) . . ? C44A C42A C43A 113.1(7) . . ? C38A C42A H42A 104.9 . . ? C44A C42A H42A 104.9 . . ? C43A C42A H42A 104.9 . . ? C42A C43A H43D 109.5 . . ? C42A C43A H43E 109.5 . . ? H43D C43A H43E 109.5 . . ? C42A C43A H43F 109.5 . . ? H43D C43A H43F 109.5 . . ? H43E C43A H43F 109.5 . . ? C42A C44A H44D 109.5 . . ? C42A C44A H44E 109.5 . . ? H44D C44A H44E 109.5 . . ? C42A C44A H44F 109.5 . . ? H44D C44A H44F 109.5 . . ? H44E C44A H44F 109.5 . . ? C61A C60A Mg1 121.1(6) . . ? C61A C60A H60C 107.0 . . ? Mg1 C60A H60C 107.0 . . ? C61A C60A H60D 107.0 . . ? Mg1 C60A H60D 107.0 . . ? H60C C60A H60D 106.8 . . ? C60A C61A C62A 118.8(9) . . ? C60A C61A H61C 107.6 . . ? C62A C61A H61C 107.6 . . ? C60A C61A H61D 107.6 . . ? C62A C61A H61D 107.6 . . ? H61C C61A H61D 107.0 . . ? C63A C62A C61A 104.1(10) . . ? C63A C62A H62C 110.9 . . ? C61A C62A H62C 110.9 . . ? C63A C62A H62D 110.9 . . ? C61A C62A H62D 110.9 . . ? H62C C62A H62D 109.0 . . ? C62A C63A H63D 109.5 . . ? C62A C63A H63E 109.5 . . ? H63D C63A H63E 109.5 . . ? C62A C63A H63F 109.5 . . ? H63D C63A H63F 109.5 . . ? H63E C63A H63F 109.5 . . ? N3 C33A C34A 116.4(4) . . ? N3 C33A C38A 123.4(4) . . ? C34A C33A C38A 120.0 . . ? C35A C34A C33A 120.0 . . ? C35A C34A C39A 118.1(5) . . ? C33A C34A C39A 121.9(5) . . ? C34A C35A C36A 120.0 . . ? C34A C35A H35A 120.0 . . ? C36A C35A H35A 120.0 . . ? C37A C36A C35A 120.0 . . ? C37A C36A H36A 120.0 . . ? C35A C36A H36A 120.0 . . ? C38A C37A C36A 120.0 . . ? C38A C37A H37A 120.0 . . ? C36A C37A H37A 120.0 . . ? C37A C38A C33A 120.0 . . ? C37A C38A C42A 116.6(5) . . ? C33A C38A C42A 122.7(5) . . ? C40A C39A C41A 112.7(10) . . ? C40A C39A C34A 113.2(8) . . ? C41A C39A C34A 110.8(8) . . ? C40A C39A H39A 106.5 . . ? C41A C39A H39A 106.5 . . ? C34A C39A H39A 106.5 . . ? C39A C40A H40D 109.5 . . ? C39A C40A H40E 109.5 . . ? H40D C40A H40E 109.5 . . ? C39A C40A H40F 109.5 . . ? H40D C40A H40F 109.5 . . ? H40E C40A H40F 109.5 . . ? C39A C41A H41D 109.5 . . ? C39A C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? C39A C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C60 Mg1 Mg2 C70 169.1(2) . . . . ? C1 Mg1 Mg2 C70 -6.40(15) . . . . ? C60A Mg1 Mg2 C70 -172.6(3) . . . . ? Cl2 Mg1 Mg2 C70 90.46(12) . . . . ? Cl1 Mg1 Mg2 C70 -95.73(12) . . . . ? C60 Mg1 Mg2 C30 -11.5(2) . . . . ? C1 Mg1 Mg2 C30 173.04(13) . . . . ? C60A Mg1 Mg2 C30 6.8(3) . . . . ? Cl2 Mg1 Mg2 C30 -90.10(11) . . . . ? Cl1 Mg1 Mg2 C30 83.71(10) . . . . ? C60 Mg1 Mg2 Cl2 78.64(19) . . . . ? C1 Mg1 Mg2 Cl2 -96.86(10) . . . . ? C60A Mg1 Mg2 Cl2 96.9(3) . . . . ? Cl1 Mg1 Mg2 Cl2 173.81(6) . . . . ? C60 Mg1 Mg2 Cl1 -95.2(2) . . . . ? C1 Mg1 Mg2 Cl1 89.33(10) . . . . ? C60A Mg1 Mg2 Cl1 -76.9(3) . . . . ? Cl2 Mg1 Mg2 Cl1 -173.81(6) . . . . ? C70 Mg2 Cl1 Mg1 114.08(10) . . . . ? C30 Mg2 Cl1 Mg1 -118.33(8) . . . . ? Cl2 Mg2 Cl1 Mg1 -4.37(4) . . . . ? C60 Mg1 Cl1 Mg2 120.71(18) . . . . ? C1 Mg1 Cl1 Mg2 -105.60(10) . . . . ? C60A Mg1 Cl1 Mg2 127.8(3) . . . . ? Cl2 Mg1 Cl1 Mg2 4.37(4) . . . . ? C60 Mg1 Cl2 Mg2 -128.98(15) . . . . ? C1 Mg1 Cl2 Mg2 100.62(8) . . . . ? C60A Mg1 Cl2 Mg2 -117.1(3) . . . . ? Cl1 Mg1 Cl2 Mg2 -4.38(5) . . . . ? C70 Mg2 Cl2 Mg1 -116.91(10) . . . . ? C30 Mg2 Cl2 Mg1 114.49(9) . . . . ? Cl1 Mg2 Cl2 Mg1 4.39(5) . . . . ? C2 N1 C1 N2 0.1(3) . . . . ? C4 N1 C1 N2 -164.0(4) . . . . ? C4A N1 C1 N2 179.6(3) . . . . ? C2 N1 C1 Mg1 177.6(2) . . . . ? C4 N1 C1 Mg1 13.5(5) . . . . ? C4A N1 C1 Mg1 -2.9(5) . . . . ? C3 N2 C1 N1 -0.1(3) . . . . ? C16 N2 C1 N1 171.8(2) . . . . ? C3 N2 C1 Mg1 -177.6(2) . . . . ? C16 N2 C1 Mg1 -5.7(4) . . . . ? C60 Mg1 C1 N1 -90.7(3) . . . . ? C60A Mg1 C1 N1 -106.3(4) . . . . ? Cl2 Mg1 C1 N1 37.6(3) . . . . ? Cl1 Mg1 C1 N1 132.6(2) . . . . ? Mg2 Mg1 C1 N1 85.6(2) . . . . ? C60 Mg1 C1 N2 86.2(3) . . . . ? C60A Mg1 C1 N2 70.6(4) . . . . ? Cl2 Mg1 C1 N2 -145.5(2) . . . . ? Cl1 Mg1 C1 N2 -50.5(2) . . . . ? Mg2 Mg1 C1 N2 -97.5(2) . . . . ? C1 N1 C2 C3 0.0(4) . . . . ? C4 N1 C2 C3 162.1(5) . . . . ? C4A N1 C2 C3 -179.6(3) . . . . ? N1 C2 C3 N2 -0.1(4) . . . . ? C1 N2 C3 C2 0.1(4) . . . . ? C16 N2 C3 C2 -172.3(3) . . . . ? C1 N1 C4 C5 82.4(6) . . . . ? C2 N1 C4 C5 -78.7(8) . . . . ? C4A N1 C4 C5 -135.9(14) . . . . ? C1 N1 C4 C9 -104.6(6) . . . . ? C2 N1 C4 C9 94.3(6) . . . . ? C4A N1 C4 C9 37.1(9) . . . . ? C9 C4 C5 C6 4.4(11) . . . . ? N1 C4 C5 C6 176.3(6) . . . . ? C9 C4 C5 C10 -178.7(7) . . . . ? N1 C4 C5 C10 -6.9(10) . . . . ? C4 C5 C6 C7 -4.6(12) . . . . ? C10 C5 C6 C7 178.6(8) . . . . ? C5 C6 C7 C8 3.9(15) . . . . ? C6 C7 C8 C9 -2.3(13) . . . . ? C5 C4 C9 C8 -3.2(11) . . . . ? N1 C4 C9 C8 -175.7(6) . . . . ? C5 C4 C9 C13 178.7(7) . . . . ? N1 C4 C9 C13 6.2(10) . . . . ? C7 C8 C9 C4 1.8(11) . . . . ? C7 C8 C9 C13 -180.0(8) . . . . ? C4 C5 C10 C11 -128.6(7) . . . . ? C6 C5 C10 C11 47.9(10) . . . . ? C4 C5 C10 C12 106.0(8) . . . . ? C6 C5 C10 C12 -77.5(9) . . . . ? C4 C9 C13 C14 145.9(8) . . . . ? C8 C9 C13 C14 -32.2(11) . . . . ? C4 C9 C13 C15 -79.4(11) . . . . ? C8 C9 C13 C15 102.6(9) . . . . ? C1 N2 C16 C21 103.4(3) . . . . ? C3 N2 C16 C21 -85.5(4) . . . . ? C1 N2 C16 C17 -80.0(4) . . . . ? C3 N2 C16 C17 91.2(3) . . . . ? C21 C16 C17 C18 0.8(5) . . . . ? N2 C16 C17 C18 -175.8(3) . . . . ? C21 C16 C17 C22 -178.4(5) . . . . ? N2 C16 C17 C22 5.1(6) . . . . ? C21 C16 C17 C22A 176.2(4) . . . . ? N2 C16 C17 C22A -0.4(5) . . . . ? C16 C17 C18 C19 1.6(6) . . . . ? C22 C17 C18 C19 -179.1(5) . . . . ? C22A C17 C18 C19 -173.1(5) . . . . ? C17 C18 C19 C20 -2.0(7) . . . . ? C18 C19 C20 C21 -0.2(7) . . . . ? C17 C16 C21 C20 -2.8(5) . . . . ? N2 C16 C21 C20 173.7(3) . . . . ? C17 C16 C21 C25 178.1(3) . . . . ? N2 C16 C21 C25 -5.4(5) . . . . ? C19 C20 C21 C16 2.5(6) . . . . ? C19 C20 C21 C25 -178.4(4) . . . . ? C18 C17 C22 C24 -31.6(8) . . . . ? C16 C17 C22 C24 147.5(6) . . . . ? C22A C17 C22 C24 170(3) . . . . ? C18 C17 C22 C23 91.2(7) . . . . ? C16 C17 C22 C23 -89.6(8) . . . . ? C22A C17 C22 C23 -68(3) . . . . ? C16 C21 C25 C27 95.0(4) . . . . ? C20 C21 C25 C27 -84.1(4) . . . . ? C16 C21 C25 C26 -143.2(3) . . . . ? C20 C21 C25 C26 37.7(5) . . . . ? C33A N3 C30 N4 169.1(4) . . . . ? C31 N3 C30 N4 -0.3(3) . . . . ? C33 N3 C30 N4 178.6(3) . . . . ? C33A N3 C30 Mg2 -24.7(5) . . . . ? C31 N3 C30 Mg2 166.0(2) . . . . ? C33 N3 C30 Mg2 -15.2(4) . . . . ? C32 N4 C30 N3 0.5(3) . . . . ? C45 N4 C30 N3 -173.5(2) . . . . ? C32 N4 C30 Mg2 -166.5(2) . . . . ? C45 N4 C30 Mg2 19.5(4) . . . . ? C70 Mg2 C30 N3 -92.4(2) . . . . ? Cl2 Mg2 C30 N3 38.1(3) . . . . ? Cl1 Mg2 C30 N3 136.1(2) . . . . ? Mg1 Mg2 C30 N3 88.1(2) . . . . ? C70 Mg2 C30 N4 71.0(3) . . . . ? Cl2 Mg2 C30 N4 -158.5(2) . . . . ? Cl1 Mg2 C30 N4 -60.5(2) . . . . ? Mg1 Mg2 C30 N4 -108.5(2) . . . . ? C33A N3 C31 C32 -169.4(4) . . . . ? C30 N3 C31 C32 0.0(4) . . . . ? C33 N3 C31 C32 -178.9(3) . . . . ? N3 C31 C32 N4 0.3(4) . . . . ? C30 N4 C32 C31 -0.5(4) . . . . ? C45 N4 C32 C31 173.4(3) . . . . ? C33A N3 C33 C34 -170(3) . . . . ? C30 N3 C33 C34 107.7(3) . . . . ? C31 N3 C33 C34 -73.5(4) . . . . ? C33A N3 C33 C38 4(3) . . . . ? C30 N3 C33 C38 -78.1(3) . . . . ? C31 N3 C33 C38 100.7(3) . . . . ? C38 C33 C34 C35 0.0 . . . . ? N3 C33 C34 C35 174.1(3) . . . . ? C38 C33 C34 C39 178.7(4) . . . . ? N3 C33 C34 C39 -7.1(4) . . . . ? C33 C34 C35 C36 0.0 . . . . ? C39 C34 C35 C36 -178.8(4) . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C33 0.0 . . . . ? C36 C37 C38 C42 176.1(4) . . . . ? C34 C33 C38 C37 0.0 . . . . ? N3 C33 C38 C37 -174.3(3) . . . . ? C34 C33 C38 C42 -176.1(4) . . . . ? N3 C33 C38 C42 9.7(4) . . . . ? C35 C34 C39 C41 -62.3(6) . . . . ? C33 C34 C39 C41 119.0(5) . . . . ? C35 C34 C39 C40 62.5(6) . . . . ? C33 C34 C39 C40 -116.3(5) . . . . ? C37 C38 C42 C43 -18.5(6) . . . . ? C33 C38 C42 C43 157.6(4) . . . . ? C37 C38 C42 C44 102.2(4) . . . . ? C33 C38 C42 C44 -81.7(5) . . . . ? C30 N4 C45 C50 -99.9(3) . . . . ? C32 N4 C45 C50 86.9(4) . . . . ? C30 N4 C45 C46 81.5(4) . . . . ? C32 N4 C45 C46 -91.8(3) . . . . ? C50 C45 C46 C47 1.8(4) . . . . ? N4 C45 C46 C47 -179.6(3) . . . . ? C50 C45 C46 C51 -174.5(3) . . . . ? N4 C45 C46 C51 4.1(4) . . . . ? C45 C46 C47 C48 -1.7(5) . . . . ? C51 C46 C47 C48 174.6(3) . . . . ? C46 C47 C48 C49 0.9(5) . . . . ? C47 C48 C49 C50 -0.1(5) . . . . ? C48 C49 C50 C45 0.1(5) . . . . ? C48 C49 C50 C54 -176.4(3) . . . . ? C46 C45 C50 C49 -1.0(4) . . . . ? N4 C45 C50 C49 -179.5(3) . . . . ? C46 C45 C50 C54 175.4(3) . . . . ? N4 C45 C50 C54 -3.1(4) . . . . ? C47 C46 C51 C53 35.6(4) . . . . ? C45 C46 C51 C53 -148.2(3) . . . . ? C47 C46 C51 C52 -88.6(4) . . . . ? C45 C46 C51 C52 87.6(4) . . . . ? C49 C50 C54 C56 -39.0(4) . . . . ? C45 C50 C54 C56 144.7(3) . . . . ? C49 C50 C54 C55 84.5(4) . . . . ? C45 C50 C54 C55 -91.8(4) . . . . ? C1 Mg1 C60 C61 -123.1(3) . . . . ? C60A Mg1 C60 C61 -23.1(13) . . . . ? Cl2 Mg1 C60 C61 110.1(3) . . . . ? Cl1 Mg1 C60 C61 5.5(4) . . . . ? Mg2 Mg1 C60 C61 61.6(4) . . . . ? Mg1 C60 C61 C62 -177.2(4) . . . . ? C60 C61 C62 C63 -179.5(5) . . . . ? C30 Mg2 C70 C71 -145.8(2) . . . . ? Cl2 Mg2 C70 C71 84.8(2) . . . . ? Cl1 Mg2 C70 C71 -19.5(2) . . . . ? Mg1 Mg2 C70 C71 33.7(3) . . . . ? Mg2 C70 C71 C72 -176.9(2) . . . . ? C70 C71 C72 C73 175.5(3) . . . . ? C1 N1 C4A C5A 88.6(4) . . . . ? C2 N1 C4A C5A -91.8(4) . . . . ? C4 N1 C4A C5A 40.8(10) . . . . ? C1 N1 C4A C9A -96.5(5) . . . . ? C2 N1 C4A C9A 83.0(4) . . . . ? C4 N1 C4A C9A -144.3(12) . . . . ? C9A C4A C5A C6A 0.0 . . . . ? N1 C4A C5A C6A 175.2(5) . . . . ? C9A C4A C5A C10A -176.4(5) . . . . ? N1 C4A C5A C10A -1.2(6) . . . . ? C4A C5A C6A C7A 0.0 . . . . ? C10A C5A C6A C7A 176.5(5) . . . . ? C5A C6A C7A C8A 0.0 . . . . ? C6A C7A C8A C9A 0.0 . . . . ? C7A C8A C9A C4A 0.0 . . . . ? C7A C8A C9A C13A -179.5(7) . . . . ? C5A C4A C9A C8A 0.0 . . . . ? N1 C4A C9A C8A -174.6(5) . . . . ? C5A C4A C9A C13A 179.5(7) . . . . ? N1 C4A C9A C13A 5.0(7) . . . . ? C6A C5A C10A C12A -62.9(7) . . . . ? C4A C5A C10A C12A 113.6(7) . . . . ? C6A C5A C10A C11A 58.9(7) . . . . ? C4A C5A C10A C11A -124.6(6) . . . . ? C8A C9A C13A C14A -42.6(11) . . . . ? C4A C9A C13A C14A 137.9(8) . . . . ? C8A C9A C13A C15A 67.3(8) . . . . ? C4A C9A C13A C15A -112.2(7) . . . . ? C18 C17 C22A C23A 87.2(9) . . . . ? C16 C17 C22A C23A -87.6(8) . . . . ? C22 C17 C22A C23A 111(3) . . . . ? C18 C17 C22A C24A -37.2(10) . . . . ? C16 C17 C22A C24A 148.0(6) . . . . ? C22 C17 C22A C24A -13(2) . . . . ? C60 Mg1 C60A C61A 159(2) . . . . ? C1 Mg1 C60A C61A -113.4(8) . . . . ? Cl2 Mg1 C60A C61A 107.2(8) . . . . ? Cl1 Mg1 C60A C61A 5.1(9) . . . . ? Mg2 Mg1 C60A C61A 52.0(9) . . . . ? Mg1 C60A C61A C62A 173.0(7) . . . . ? C60A C61A C62A C63A 81.7(13) . . . . ? C30 N3 C33A C34A 97.4(4) . . . . ? C31 N3 C33A C34A -94.5(5) . . . . ? C33 N3 C33A C34A -6(3) . . . . ? C30 N3 C33A C38A -77.8(5) . . . . ? C31 N3 C33A C38A 90.4(5) . . . . ? N3 C33A C34A C35A -175.3(6) . . . . ? C38A C33A C34A C35A 0.0 . . . . ? N3 C33A C34A C39A 5.8(7) . . . . ? C38A C33A C34A C39A -178.9(7) . . . . ? C33A C34A C35A C36A 0.0 . . . . ? C39A C34A C35A C36A 178.9(7) . . . . ? C34A C35A C36A C37A 0.0 . . . . ? C35A C36A C37A C38A 0.0 . . . . ? C36A C37A C38A C33A 0.0 . . . . ? C36A C37A C38A C42A -171.0(6) . . . . ? N3 C33A C38A C37A 175.0(7) . . . . ? C34A C33A C38A C37A 0.0 . . . . ? N3 C33A C38A C42A -14.6(7) . . . . ? C34A C33A C38A C42A 170.4(7) . . . . ? C44A C42A C38A C37A -70.1(7) . . . . ? C43A C42A C38A C37A 61.5(8) . . . . ? C44A C42A C38A C33A 119.2(7) . . . . ? C43A C42A C38A C33A -109.2(7) . . . . ? C35A C34A C39A C40A 45.1(11) . . . . ? C33A C34A C39A C40A -135.9(8) . . . . ? C35A C34A C39A C41A -82.6(9) . . . . ? C33A C34A C39A C41A 96.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.649 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.054 #===END #===END data_nBuMgHMDS _database_code_depnum_ccdc_archive 'CCDC 775967' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H54 Mg2 N2 Si4' _chemical_formula_sum 'C20 H54 Mg2 N2 Si4' _chemical_formula_weight 483.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.3833(5) _cell_length_b 11.1092(3) _cell_length_c 17.1805(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.001(3) _cell_angle_gamma 90.00 _cell_volume 3125.04(16) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7374 _cell_measurement_theta_min 3.2084 _cell_measurement_theta_max 30.2143 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85798 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11966 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 30.28 _reflns_number_total 4261 _reflns_number_gt 3413 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+3.5350P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4261 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.04308(3) 0.69432(5) 0.17336(3) 0.02345(13) Uani 1 1 d . . . Si2 Si 0.06920(3) 0.25951(4) 0.19551(3) 0.02145(13) Uani 1 1 d . . . Mg1 Mg 0.06838(4) 0.47920(6) 0.30593(3) 0.02084(15) Uani 1 1 d . . . N1 N 0.0000 0.34136(18) 0.2500 0.0192(4) Uani 1 2 d S . . N2 N 0.0000 0.61721(19) 0.2500 0.0198(4) Uani 1 2 d S . . C1 C 0.11230(13) 0.12420(18) 0.24739(12) 0.0323(4) Uani 1 1 d . . . H1A H 0.1492 0.0815 0.2132 0.048 Uiso 1 1 calc R . . H1B H 0.0677 0.0705 0.2614 0.048 Uiso 1 1 calc R . . H1C H 0.1426 0.1498 0.2947 0.048 Uiso 1 1 calc R . . C4 C 0.03534(13) 0.59484(18) 0.08463(10) 0.0284(4) Uani 1 1 d . . . H4A H -0.0207 0.5965 0.0629 0.043 Uiso 1 1 calc R . . H4B H 0.0499 0.5121 0.0993 0.043 Uiso 1 1 calc R . . H4C H 0.0728 0.6241 0.0456 0.043 Uiso 1 1 calc R . . C10 C 0.17490(13) 0.4706(2) 0.37829(13) 0.0357(5) Uani 1 1 d . . . C3 C 0.16148(12) 0.3545(2) 0.17722(13) 0.0343(5) Uani 1 1 d . . . H3A H 0.1930 0.3176 0.1360 0.051 Uiso 1 1 calc R . . H3B H 0.1956 0.3600 0.2251 0.051 Uiso 1 1 calc R . . H3C H 0.1440 0.4353 0.1610 0.051 Uiso 1 1 calc R . . C2 C 0.02162(14) 0.2136(2) 0.09937(12) 0.0359(5) Uani 1 1 d . . . H2A H 0.0642 0.1846 0.0653 0.054 Uiso 1 1 calc R . . H2B H -0.0061 0.2829 0.0751 0.054 Uiso 1 1 calc R . . H2C H -0.0181 0.1492 0.1074 0.054 Uiso 1 1 calc R . . C11 C 0.19646(14) 0.5675(2) 0.43724(13) 0.0396(5) Uani 1 1 d . . . H11A H 0.1551 0.5669 0.4779 0.047 Uiso 1 1 calc R . . H11B H 0.1931 0.6466 0.4108 0.047 Uiso 1 1 calc R . . C5 C -0.01188(18) 0.83492(19) 0.14323(13) 0.0437(6) Uani 1 1 d . . . H5A H -0.0085 0.8934 0.1859 0.066 Uiso 1 1 calc R . . H5B H -0.0693 0.8162 0.1307 0.066 Uiso 1 1 calc R . . H5C H 0.0134 0.8690 0.0973 0.066 Uiso 1 1 calc R . . C6 C 0.15254(15) 0.7302(2) 0.19642(14) 0.0449(6) Uani 1 1 d . . . H6A H 0.1563 0.7854 0.2409 0.067 Uiso 1 1 calc R . . H6B H 0.1766 0.7684 0.1511 0.067 Uiso 1 1 calc R . . H6C H 0.1822 0.6559 0.2093 0.067 Uiso 1 1 calc R . . C12 C 0.28148(15) 0.5554(3) 0.47717(15) 0.0553(8) Uani 1 1 d . . . H12A H 0.3227 0.5538 0.4364 0.066 Uiso 1 1 calc R . . H12B H 0.2920 0.6282 0.5093 0.066 Uiso 1 1 calc R . . C13 C 0.29383(19) 0.4477(3) 0.52751(17) 0.0665(9) Uani 1 1 d . . . H13A H 0.3489 0.4497 0.5517 0.100 Uiso 1 1 calc R . . H13B H 0.2874 0.3747 0.4959 0.100 Uiso 1 1 calc R . . H13C H 0.2534 0.4478 0.5682 0.100 Uiso 1 1 calc R . . H10A H 0.1877(17) 0.394(3) 0.4142(17) 0.058(8) Uiso 1 1 d . . . H10B H 0.218(2) 0.469(3) 0.3444(19) 0.070(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0270(3) 0.0210(2) 0.0222(2) 0.00273(18) -0.00161(19) -0.0030(2) Si2 0.0223(2) 0.0210(2) 0.0210(2) 0.00083(18) 0.00020(17) 0.00390(19) Mg1 0.0183(3) 0.0214(3) 0.0224(3) 0.0002(2) -0.0051(2) 0.0001(2) N1 0.0182(10) 0.0179(9) 0.0214(9) 0.000 -0.0010(7) 0.000 N2 0.0199(10) 0.0199(10) 0.0192(9) 0.000 -0.0026(7) 0.000 C1 0.0328(11) 0.0265(10) 0.0375(11) 0.0055(8) -0.0005(8) 0.0089(8) C4 0.0334(10) 0.0306(10) 0.0212(8) -0.0002(7) 0.0004(7) 0.0017(8) C10 0.0247(10) 0.0485(13) 0.0331(10) -0.0039(10) -0.0095(8) 0.0041(9) C3 0.0239(10) 0.0374(11) 0.0418(11) 0.0068(9) 0.0068(8) 0.0034(8) C2 0.0378(12) 0.0456(12) 0.0243(9) -0.0054(9) -0.0017(8) 0.0092(10) C11 0.0353(12) 0.0444(13) 0.0381(11) 0.0000(10) -0.0109(9) -0.0052(10) C5 0.0735(18) 0.0233(10) 0.0342(11) 0.0051(8) -0.0007(11) 0.0078(11) C6 0.0362(12) 0.0587(15) 0.0397(12) 0.0049(11) -0.0001(10) -0.0235(11) C12 0.0309(12) 0.097(2) 0.0372(12) -0.0001(14) -0.0104(10) -0.0161(14) C13 0.0495(16) 0.101(3) 0.0478(15) 0.0028(16) -0.0145(13) 0.0155(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N2 1.7408(11) . ? Si1 C6 1.866(2) . ? Si1 C5 1.867(2) . ? Si1 C4 1.8836(19) . ? Si1 Mg1 3.0361(8) 2 ? Si2 N1 1.7500(12) . ? Si2 C2 1.872(2) . ? Si2 C1 1.8731(19) . ? Si2 C3 1.879(2) . ? Si2 Mg1 3.0915(8) . ? Mg1 N1 2.1090(16) . ? Mg1 C10 2.109(2) . ? Mg1 N2 2.1104(16) . ? Mg1 Mg1 2.9005(11) 2 ? Mg1 Si1 3.0361(8) 2 ? N1 Si2 1.7500(12) 2 ? N1 Mg1 2.1090(16) 2 ? N2 Si1 1.7408(11) 2 ? N2 Mg1 2.1105(16) 2 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C10 C11 1.512(3) . ? C10 H10A 1.07(3) . ? C10 H10B 0.92(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C11 C12 1.537(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C12 C13 1.486(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Si1 C6 110.90(8) . . ? N2 Si1 C5 114.65(10) . . ? C6 Si1 C5 109.30(12) . . ? N2 Si1 C4 107.80(9) . . ? C6 Si1 C4 109.53(11) . . ? C5 Si1 C4 104.37(10) . . ? C6 Si1 Mg1 136.13(9) . 2 ? C5 Si1 Mg1 113.88(9) . 2 ? C4 Si1 Mg1 66.99(7) . 2 ? N1 Si2 C2 110.85(7) . . ? N1 Si2 C1 113.76(8) . . ? C2 Si2 C1 109.85(10) . . ? N1 Si2 C3 109.74(9) . . ? C2 Si2 C3 108.54(11) . . ? C1 Si2 C3 103.77(10) . . ? C2 Si2 Mg1 138.23(7) . . ? C1 Si2 Mg1 110.56(7) . . ? C3 Si2 Mg1 71.35(7) . . ? N1 Mg1 C10 130.62(8) . . ? N1 Mg1 N2 93.15(6) . . ? C10 Mg1 N2 135.76(8) . . ? N1 Mg1 Mg1 46.56(4) . 2 ? C10 Mg1 Mg1 174.06(8) . 2 ? N2 Mg1 Mg1 46.59(4) . 2 ? N1 Mg1 Si1 108.23(4) . 2 ? C10 Mg1 Si1 117.08(7) . 2 ? N2 Mg1 Si1 33.86(2) . 2 ? Mg1 Mg1 Si1 67.903(18) 2 2 ? N1 Mg1 Si2 32.95(2) . . ? C10 Mg1 Si2 107.74(7) . . ? N2 Mg1 Si2 107.92(4) . . ? Mg1 Mg1 Si2 67.244(17) 2 . ? Si1 Mg1 Si2 135.14(2) 2 . ? Si2 N1 Si2 117.39(12) 2 . ? Si2 N1 Mg1 118.50(3) 2 . ? Si2 N1 Mg1 106.10(3) . . ? Si2 N1 Mg1 106.10(3) 2 2 ? Si2 N1 Mg1 118.50(3) . 2 ? Mg1 N1 Mg1 86.89(8) . 2 ? Si1 N2 Si1 121.04(12) 2 . ? Si1 N2 Mg1 118.63(4) 2 2 ? Si1 N2 Mg1 103.64(3) . 2 ? Si1 N2 Mg1 103.64(3) 2 . ? Si1 N2 Mg1 118.63(4) . . ? Mg1 N2 Mg1 86.81(8) 2 . ? Si2 C1 H1A 109.5 . . ? Si2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C11 C10 Mg1 122.13(16) . . ? C11 C10 H10A 98.2(15) . . ? Mg1 C10 H10A 121.3(16) . . ? C11 C10 H10B 106(2) . . ? Mg1 C10 H10B 105(2) . . ? H10A C10 H10B 102(2) . . ? Si2 C3 H3A 109.5 . . ? Si2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C2 H2A 109.5 . . ? Si2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C10 C11 C12 115.1(2) . . ? C10 C11 H11A 108.5 . . ? C12 C11 H11A 108.5 . . ? C10 C11 H11B 108.5 . . ? C12 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C13 C12 C11 115.6(2) . . ? C13 C12 H12A 108.4 . . ? C11 C12 H12A 108.4 . . ? C13 C12 H12B 108.4 . . ? C11 C12 H12B 108.4 . . ? H12A C12 H12B 107.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Si2 Mg1 N1 61.65(13) . . . . ? C1 Si2 Mg1 N1 -102.96(10) . . . . ? C3 Si2 Mg1 N1 158.89(10) . . . . ? N1 Si2 Mg1 C10 139.75(10) . . . . ? C2 Si2 Mg1 C10 -158.60(14) . . . . ? C1 Si2 Mg1 C10 36.79(11) . . . . ? C3 Si2 Mg1 C10 -61.36(11) . . . . ? N1 Si2 Mg1 N2 -66.87(7) . . . . ? C2 Si2 Mg1 N2 -5.22(13) . . . . ? C1 Si2 Mg1 N2 -169.83(8) . . . . ? C3 Si2 Mg1 N2 92.02(8) . . . . ? N1 Si2 Mg1 Mg1 -43.63(6) . . . 2 ? C2 Si2 Mg1 Mg1 18.02(12) . . . 2 ? C1 Si2 Mg1 Mg1 -146.59(8) . . . 2 ? C3 Si2 Mg1 Mg1 115.26(7) . . . 2 ? N1 Si2 Mg1 Si1 -42.69(7) . . . 2 ? C2 Si2 Mg1 Si1 18.96(13) . . . 2 ? C1 Si2 Mg1 Si1 -145.65(8) . . . 2 ? C3 Si2 Mg1 Si1 116.20(8) . . . 2 ? C2 Si2 N1 Si2 83.71(9) . . . 2 ? C1 Si2 N1 Si2 -40.67(8) . . . 2 ? C3 Si2 N1 Si2 -156.41(8) . . . 2 ? Mg1 Si2 N1 Si2 -135.15(5) . . . 2 ? C2 Si2 N1 Mg1 -141.14(9) . . . . ? C1 Si2 N1 Mg1 94.48(10) . . . . ? C3 Si2 N1 Mg1 -21.26(9) . . . . ? C2 Si2 N1 Mg1 -45.84(12) . . . 2 ? C1 Si2 N1 Mg1 -170.21(9) . . . 2 ? C3 Si2 N1 Mg1 74.04(9) . . . 2 ? Mg1 Si2 N1 Mg1 95.30(11) . . . 2 ? C10 Mg1 N1 Si2 80.39(12) . . . 2 ? N2 Mg1 N1 Si2 -106.65(7) . . . 2 ? Mg1 Mg1 N1 Si2 -106.65(7) 2 . . 2 ? Si1 Mg1 N1 Si2 -75.68(8) 2 . . 2 ? Si2 Mg1 N1 Si2 134.55(12) . . . 2 ? C10 Mg1 N1 Si2 -54.17(11) . . . . ? N2 Mg1 N1 Si2 118.80(6) . . . . ? Mg1 Mg1 N1 Si2 118.80(6) 2 . . . ? Si1 Mg1 N1 Si2 149.77(5) 2 . . . ? C10 Mg1 N1 Mg1 -172.96(11) . . . 2 ? N2 Mg1 N1 Mg1 0.0 . . . 2 ? Si1 Mg1 N1 Mg1 30.968(15) 2 . . 2 ? Si2 Mg1 N1 Mg1 -118.80(6) . . . 2 ? C6 Si1 N2 Si1 87.30(10) . . . 2 ? C5 Si1 N2 Si1 -37.06(9) . . . 2 ? C4 Si1 N2 Si1 -152.80(7) . . . 2 ? Mg1 Si1 N2 Si1 -136.18(5) 2 . . 2 ? C6 Si1 N2 Mg1 -136.52(10) . . . 2 ? C5 Si1 N2 Mg1 99.12(11) . . . 2 ? C4 Si1 N2 Mg1 -16.62(9) . . . 2 ? C6 Si1 N2 Mg1 -42.66(14) . . . . ? C5 Si1 N2 Mg1 -167.02(10) . . . . ? C4 Si1 N2 Mg1 77.24(9) . . . . ? Mg1 Si1 N2 Mg1 93.86(12) 2 . . . ? N1 Mg1 N2 Si1 118.70(6) . . . 2 ? C10 Mg1 N2 Si1 -68.95(12) . . . 2 ? Mg1 Mg1 N2 Si1 118.70(6) 2 . . 2 ? Si2 Mg1 N2 Si1 148.77(5) . . . 2 ? N1 Mg1 N2 Si1 -103.81(8) . . . . ? C10 Mg1 N2 Si1 68.53(13) . . . . ? Mg1 Mg1 N2 Si1 -103.81(8) 2 . . . ? Si1 Mg1 N2 Si1 137.48(13) 2 . . . ? Si2 Mg1 N2 Si1 -73.75(8) . . . . ? N1 Mg1 N2 Mg1 0.0 . . . 2 ? C10 Mg1 N2 Mg1 172.34(11) . . . 2 ? Si1 Mg1 N2 Mg1 -118.70(6) 2 . . 2 ? Si2 Mg1 N2 Mg1 30.061(15) . . . 2 ? N1 Mg1 C10 C11 -155.35(16) . . . . ? N2 Mg1 C10 C11 34.7(3) . . . . ? Si1 Mg1 C10 C11 -1.0(2) 2 . . . ? Si2 Mg1 C10 C11 177.07(18) . . . . ? Mg1 C10 C11 C12 -172.22(18) . . . . ? C10 C11 C12 C13 -65.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.694 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.062